Category: 7252-83-7

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, A new synthetic method of this compound is introduced below., category: ethers-buliding-blocks

[000398] A mixture of Compound 24A (10 g, 89 mmol), 2-bromo-l,l- dimethoxyethane(15 g, 89 mmol), K2C03 (18.4 g, 134 mmol), KI (100 mg) in DMF (100 mL) was stirred at reflux for 3 h, then cooled to rt, and filtered. The filtrate was added water (200 mL), extracted with ethyl acetate (100 mL x 2), washed with water (100 mL x 3), brine (100 mL x 1), dried over Na2S04, concentrated, and purified by silica gel column chromatography (ethyl acetate in petroleum ether, 10% v/v) to render Compound 24B (15 g, yield 85%>) as a colorless liquid. 1H-NMR (CDC13, 400 MHz) major characteristic peaks: delta (ppm) 3.46 (s, 6H), 3.96 (d, J= 5.2 Hz, 2H), 4.71 (t, J= 5.6 Hz, 1H), 6.90 (m, 2H), 7.26 (m, 2H).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; BIOMARIN PHARMACEUTICAL INC.; WANG, Bing; CHU, Daniel; BRIDGES, Alexander, James; WO2015/42397; (2015); A1;,
Ether – Wikipedia,
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In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 2-Bromo-1,1-dimethoxyethane

As described by Doel et al.,13 a solution of adenine or thymine (1 equiv) and K2CO3 (1 equiv) in DMF (10 mL) was stirred at 100 C in the presence of 2-bromo-1,1-dimethoxyethane (1.1 equiv). After 24 h, the reaction was filtered and the solvent removed under reduced pressure. The crude mixture was purified by column chromatography in silica gel with MeOH: CH2Cl2 or EtOAc: hexane as mobile phase. Corresponding 9-(2,2-dimethoxyethyl)-adenine and 1-(2,2-dimethoxyethyl)-thymine were obtained in 61% and 38% isolated yields respectively. Both acetals were completely hydrolyzed after 1 h stirring in HCl 1 N at 90 C, to yield the corresponding aldehydes.20

The synthetic route of 7252-83-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Palazzolo, Martin A.; Perez-Sanchez, Maria; Dominguez De Maria, Pablo; Iribarren, Adolfo M.; Lewkowicz, Elizabeth S.; Tetrahedron Letters; vol. 53; 50; (2012); p. 6797 – 6800,4;,
Ether – Wikipedia,
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Some common heterocyclic compound, 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, molecular formula is C4H9BrO2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. SDS of cas: 7252-83-7

[000321] A mixture of 4-chlorophenol (10 g, 78 mmol), 2-bromo-l,l- dimethoxyethane(13.1 g, 78 mmol), K2C03 (14 g, 101 mmol), KI (100 mg) in DMF (50 mL) was stirred at reflux for 3 h. The mixture was cooled to rt and filtered. The filtrate was added water (200 mL), extracted with ethyl acetate (100 mL x 2), washed with water (100 mL x 3), brine (100 mL x 1), dried over Na2S04, concentrated, and purified by column chromatography on silica gel (ethyl acetate in petroleum ether, 10% v/v) to yield Compound 11A (15 g, yield 89 %) as a colorless liquid. 1H-NMR (CDC13, 400 MHz) major characteristic peaks: delta (ppm) 3.45 (s, 6H), 3.96 (d, J= 5.2 Hz, 2H), 4.70 (t, J= 5.6 Hz, 1H), 6.85 (d, J= 8.8 Hz, 2H), 7.21 (d, J= 8.8 Hz, 2H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 7252-83-7, its application will become more common.

Reference:
Patent; BIOMARIN PHARMACEUTICAL INC.; WANG, Bing; CHU, Daniel; BRIDGES, Alexander, James; WO2015/42397; (2015); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Reference of 7252-83-7, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A 100-mL, three-neck flask was charged with 2-bromo-l,l-dimethoxyethane 4 (23.2 g (16 mL, 137.2 mmol) and aqueous HBr (47.6% HBr by wt, 8.8 mmol/mL, 6.6 mL, 58.8 mmol), and the reaction mixture was heated to reflux (55C) for 2 hours. The mixture was allowed to cool to 40C, and solid NaHCC3 was added in small portions, until evolution of gas ceased. The resulting suspension was filtered, under vacuum, into a 500-mL, three-neck flask, and the filter cake was washed with isopropanol (200 mL). Solid 3,5-dibromopyrazin-2-amine (3) (12.0 g, 47.2 mmol) was added into the isopropanol filtrate, and the reaction mixture was heated at reflux (78C) for 16 hours. The resulting suspension was cooled to room temperature, filtered, the cake was washed with cold isopropanol (100 mL), and then the cake was dried under vacuum. The cake was transferred into a three-neck flask, into which, water (200 mL) was added, followed by solid K2CC3, in small portions, until gas evolution ceased, after which the reaction was stirred for 30 minutes. The resulting precipitate was isolated by filtration, and washed with water (200 mL). The solid was dried at 50C, to constant weight, then dissolved in THF, filtered through a plug (celite, silica gel, and charcoal). The solvent was removed under vacuum, to give 12.0 g of the desired product (5) as a white solid at 99% purity, as determined by NMR and LC-MS. IH NMR (500 MHz, CDC13) delta 8.26 (s, IH), 7.84 (d, J = 1.0 Hz, IH), 7.78 (d, J = 1.1 Hz, IH); 13C NMR (126 MHz, CDC13) delta 136.93, 134.06, 120.29, 119.26, 115.78.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2-Bromo-1,1-dimethoxyethane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; DOW GLOBAL TECHNOLOGIES LLC; ROHM AND HAAS ELECTRONIC MATERIALS KOREA LTD.; ONDARI, Mark E.; WELSH, Dean M.; FROESE, Robert DJ; NA, Hong-Yeop; (38 pag.)WO2016/209895; (2016); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Electric Literature of 7252-83-7,Some common heterocyclic compound, 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, molecular formula is C4H9BrO2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

To a stirred solution of 3-bromothiophenol (10.0 g, 52.88 mmol) in DMF (180 mL) was added NaH (3.0 g, 63.45 mmol) portionwise at 0C. After the addition, the reaction mixture was stirred at room temperature for 30 mi Bromoacetaldehyde dimethylacetal (6.85 mL, 58.17 mmol) was added dropwise and the resulting mixture was stirred at room temperature for 2 hr. The reaction mixture was diluted with EtOAc (250 mL) and washed with cold water and brine solution. The organic layer was dried over anhydrous sodium sulfate, concentrated under reduced pressure to afford the crude material which was purified by column chromatography using silica gel (100-200 mesh) and 2% EtOAc-hexane as eluent to afford 1-bromo-3-(2,2-dimethoxy- ethylsulphanyl)-benzene (11.0 g, 36.038 mmol, 68%) as colorless liquid. GCMS: 277 (mlz).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Bromo-1,1-dimethoxyethane, its application will become more common.

Reference:
Patent; CURADEV PHARMA PRIVATE LTD.; BANERJEE, Monali; MIDDYA, Sandip; SHRIVASTAVA, Ritesh; RAINA, Sushil; SURYA, Arjun; YADAV, Dharmendra B.; YADAV, Veejendra K.; KAPOOR, Kamal Kishore; VENKATESAN, Aranapakam; SMITH, Roger A.; THOMPSON, Scott K.; WO2014/186035; (2014); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Electric Literature of 7252-83-7,Some common heterocyclic compound, 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, molecular formula is C4H9BrO2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Step 1: Synthesis of 2-chloro-7-(2,2-dimethoxyethyl)-4-morpholin-4-yl-7H-pyrrolo[2,3-d]pyrimidine To a solution of 2-chloro-4-morpholin-4-yl-7H-pyrrolo[2,3-d]pyrimidine (650 mg, 2.7 mmol) in DMF (10 mL) were added 2-bromo-1,1-dimethoxyethane (0.65 mL, 5.4 mmol) and Cs2CO3 (1.067 g, 3.3 mmol). The resulting mixture was heated at 80 C. under nitrogen overnight, and cooled to room temperature. Water was added, and the mixture was extracted with EtOAc. The combined extracts were washed with water and brine, dried over MgSO4. The solvent was removed under reduced pressure to give the title compound as light yellow solid (665 mg, 75% yield), which was used in next step without further purification. MS(ESI) m/z 327.2.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Bromo-1,1-dimethoxyethane, its application will become more common.

Reference:
Patent; Wyeth; US2010/3250; (2010); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Adding a certain compound to certain chemical reactions, such as: 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, belongs to ethers-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 7252-83-7, Application In Synthesis of 2-Bromo-1,1-dimethoxyethane

Dissolve 4-fluorophenol (5.5 g, 49.1 mmol) in acetonitrile (49 mL) and treat the solution with 2-bromo-l, l-dimethoxy ethane (11.6 mL, 98.1 mmol) and K2CO3 (16.95 g, 122.7 mmol). Heat the solution to reflux with stirring for five days. Filter the mixture, and concentrate the filtrate under reduced pressure. Subject the resulting crude material to silica gel chromatography eluting with a gradient of 0% to 50% EtOAc/hexanes. Concentrate the fractions containing the desired product under reduced pressure to furnish the title compound as a colorless oil (5.85 g, 60% yield). Mass spectrum (m/z) 218 (M + NH4)+, 223 (M + Na)+.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2-Bromo-1,1-dimethoxyethane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ELI LILLY AND COMPANY; SCHIFFLER, Matthew Allen; YORK, Jeremy Schulenburg; WO2014/4229; (2014); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Adding a certain compound to certain chemical reactions, such as: 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, belongs to ethers-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 7252-83-7, Recommanded Product: 2-Bromo-1,1-dimethoxyethane

To a mixture of 4-chloro-6-aminobenzene-1,3-disulfonamide (Aldrich, 15.2 g, 53.3 mmol) and bromoacetaldehyde dimethylacetal (6.3 mL, 9 g, 53.3 mmol) in anhydrous dioxane (45 mL) at 120 C., was added dropwise 48% hydrobromic acid in H20 (2 mL). The mixture was then heated at 100 C. for 20 minutes. The residue, after evaporation of the solvent, was diluted with water, the resultant precipitate was filtered, washed with water to give a sticky solid that was dissolved in EtOAc and dried over Na2SO4. The residue after evaporation of the solvent was recrystallized from EtOAc/hexane to give the title compound in quantitative yield as a white solid: mp 203-205 C.; 1H NMR (400 MHz, d6-DMSO) delta 8.16 (br s, 1H), 8.08 (br d, J=11.2Hz, 1H), 7.99 (s, 1H), 7.53 (br s, 2H), 7.05 (s, 1H), 4.88-5.03 (m, 1H), 3.65-3.72 (m, 2H); 13C NMR (100 MHz, d6-DMSO) delta 146.1, 134.7, 128.9, 125.3, 118.4, 117.4, 66.3, 31.5; Mass spectrum (API-TIS) m/z 387/389 (M-H), 407/409 (MNH4+); Anal. calcd for C8H9BrClN3O4S2. EtOAc: C, 25.41; H, 2.50; N, 10.46; Found: C, 25.35; H, 2.44; N, 10.46.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Bromo-1,1-dimethoxyethane, and friends who are interested can also refer to it.

Reference:
Patent; NitroMed, Inc.; US2006/189603; (2006); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Adding a certain compound to certain chemical reactions, such as: 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, belongs to ethers-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 7252-83-7, category: ethers-buliding-blocks

i. Preparation of compound 311. 1-(2-Amino-3-chloro-4-hydroxy-phenyl)-ethanone 310 (40 g, 215 mmol) was dissolved in DMF (360 ml). Cesium carbonate (140 g, 430 mmol) was added, followed by bromoacetaldehyde dimethyl acetal (54.5 g, 323 mmol). The mixture was then vigorously stirred at 65 C for 24 hours. Upon cooling to room temperature, EtOAc (1 L) and H20 (1 L) were added to the mixture. The organic layer was extracted with EtOAc (1 x 400 ml). The combined organic layer was washed with aqueous 3% LiCI solution (2 x 1 L), brine, dried (Na2S04) and concentrated in vacuo. The residue was purified by silica gel chromatography to give compound 311 as a white solid (39 g, 67%).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; GILEAD SCIENCES, INC.; RAY, Adrian S.; WATKINS, William J.; LINK, John O.; OLDACH, David W.; DELANEY, IV, William E.; WO2013/40492; (2013); A2;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Electric Literature of 7252-83-7, These common heterocyclic compound, 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Example 31 [000431] A mixture of Compound 31A (3.00 g, 14.93 mmol), 2-bromo-l,l- dimethoxyethane (2.77 g, 16.42 mmol) and K2C03 (4.12 g, 29.86 mmol) in DMF (26 mL) was stirred at 150 C for 2 h. It was evaporated to remove DMF. The residue was diluted with ethyl acetate (200 mL), washed with water and brine, dried with anhydrous Na2S04, and evaporated to render Compound 31B (3.80 g, yield 88%) as a white solid. 1H-NMR (CDC13, 400 MHz) major characteristic peaks: delta (ppm) 4.10 (d, J= 5.2 Hz, 2H), 4.75 (t, J= 5.2 Hz, 1H), 6.89 (d, J= 9.2 Hz, 1H), 7.61-7.64 (m, 1H), 7.93 (s, 1H), 10.42 (s, 1H).

The synthetic route of 7252-83-7 has been constantly updated, and we look forward to future research findings.

Reference:
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem