Category: 7252-83-7

Synthetic Route of 7252-83-7, A common heterocyclic compound, 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, molecular formula is C4H9BrO2, 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.

[0252] Part A: A suspension of 3-bromothiophenol (15.2 g, 81 mmol), bromoacetaldehyde dimethylacetal (9.5 mL, 81 mmol) and potassium carbonate (12.2 g, 88 mmol) in acetone (90 mL) was stirred at ambient temperature overnight. The solid was filtered and rinsed with ether. Evaporation of the filtrate afforded 23 g of 1-bromo-3-((2,2-dimethoxyethyl)thio)benzene which was carried forward without further purification.

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; O’Connor, Stephen P.; Lawrence, Michael; Shi, Yan; Stein, Philip D.; US2004/186134; (2004); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Application of 7252-83-7, A common heterocyclic compound, 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, molecular formula is C4H9BrO2, 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.

2-[3,6-Bis-(2,2-dimethoxy-ethoxy)-2,7-difluoro-9H-xanthen-9-yl]-benzoic acid 2,2-dimethoxy-ethyl ester (Compound 102) Acid 101 (all material prepared in the previous step, ~10.9 mmol) was dissolved in 150 mL of DMF. Powdered K2CO3 (25 g, 180 mmol) was added to the solution followed by adding of bromoacetaldehyde dimethyl acetal (33.3. mL, 283 mmol). The reaction mixture was stirred overnight at 110 C. DMF solution was removed from the flask (leaving insoluble material in the flask) and evaporated. The residue was mixed with 150 mL of water and combined with the solid left in the flask. The product was extracted with ethyl acetate (4*45 mL), combined extracts were washed with water (4*30 mL), brine (30 mL), dried over sodium sulfate and evaporated in vacuum. The residue was dissolved in chloroform, loaded on silica gel column (packed in 100:3 chloroform-EtOAc mixture). The column was eluted with 100:3 chloroform-EtOAc mixture. Pure fractions containing the product were combined and evaporated to give ester 102 as a clear oil, solidified later to form white solid (4.54 g, 66%).

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

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. Recommanded Product: 7252-83-7

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.

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.

In a 250 mL round bottom flask was added 4-(morpholinyl)thiobenzamide (2.22 g, 10 mmol) and dissolved in ethanol (50 mL).Then 2-bromo-1,1-dimethoxyethane (1.69 g, 10 mmol) and p-toluenesulfonic acid (1.90 g, 10 mmol) were added while stirring, and the reaction system was heated to 95C and reacted overnight.After the reaction was completed, the mixture was cooled to room temperature and filtered to give a solid which after drying gave a yellow solid (2.00 g, 81%).

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

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 7252-83-7

A solution of 6-chloro-1,2-diazinan-3-amine (10 g, 73.75 mmol, l.OOequiv), 2-bromo-1,1-dimethoxyethane (50 g, 295.83 mmol, 4.01 equiv), and HBr(40%, 45 mL) in ethanol (100 mL) was stirred overnight at 90 C. The majority of the ethanol was removed under reduced pressure then the pH value of the solution was adjusted to 10 with 5% aqueous potassium carbonate solution. The resulting mixture was extracted with 6×500 mL of ethyl acetate. The combined organic layers were dried over anhydrous sodium sulfate and concentrated under vacuum. The residue was purified on a silica gel column eluted with ethyl acetate/petroleum ether (1/2-1/1) to give 6,5 g (57%) of the title compound as a yellow solid. 1H NMR (300 MHz, CDCl3) delta 7.95 (s, 1 H), 7.91 (s, 1H), 7.80 (s, 1 H), 7.05 (d,.7 = 9.3 Hz, 1 H).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 7252-83-7.

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, This compound has unique chemical properties. The synthetic route is as follows., name: 2-Bromo-1,1-dimethoxyethane

To an aqueous (10 kg) solution of 3,5-dibromopyrazine-2-amine (1018 g, 4.03 mol), 2-bromo-1,1-dimethoxyethane (1.79 kg, 4.14 mol) was added at room temperature and stirred for 2 hours while heating under reflux. To the reaction solution, water (15.3 kg) and sodium hydrogen carbonate (744 g) were added and further stirred for 15 minutes. The resultant solid substance was obtained by filtration to obtain the titled compound (1106 g, 3.99 mmol, 99%) as a brown solid substance.1H-NMR (400 MHz, DMSO-d6) delta 7.90 (s, 1H), 8.23 (s, 1H), 9.02 (s, 1H).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes 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. Application In Synthesis of 2-Bromo-1,1-dimethoxyethane

Example 1. (2S)-4-Methyl-2-[(1R, 5S, 7S)-2-oxo-7-(piperidine-1-carbonyl)-6,8-dioxa-3-aza-bicyclo[3.2.1]oct-3-yl]-pentanoic acid methyl ester [compound formula (I), where R1 = -CH(Leu side chain)COOCH3, R2 = H, R3 and R4 = – CH2(CH2)3CH2-] A solution containing L-leucine methyl ester hydrochloride (2.9 g, 16 mmol), 2-bromo-1,1-dimethoxy ethane (1.9 ml, 2.7 g, 16 mmol), NEt3 (6.7 ml, 48 mmol) and a catalytic amount of KI in DMF (190 ml) was stirred at 120 C for 3 days. The reaction mixture was concentrated under reduced pressure, diluted with water and extracted with DCM. The organic layer was then washed with brine, dried over Na2SO4 and evaporated. The crude product was purified by column chromatography (silica gel, EtOAc/P.E. 1:1) to afford compound of formula (III), where R = Leu side chain, as a yellow oil (1.2 g, 32% yield). [alpha]D24 -3.32 (c 1.0, CHCl3); 1H-NMR (CDCl3, 200 MHz): delta 4.38 (t, J = 6 Hz, 1H), 3.65 (s, 3H), 3.30 (s, 3H), 3.29 (s, 3H), 3.24 (t, J = 6 Hz, 1H), 2.68 (dd, J1 = J2 = 6 Hz, 1H), 2.52 (dd, J1 = J2 = 6 Hz, 1H), 1.71-1.55 (m, 2H), 1.44-1.37 (m, 2H), 0.86 (d, J = 4 Hz, 3H), 0.83 (d, J = 4 Hz, 3H); 13C-NMR (CDCl3, 200 MHz): delta 175.9 (s), 103.6 (d), 59.9 (d), 54.0 (q), 53.1 (q), 51.7 (q), 49.3 (t), 42.8 (t), 25.0 (d), 22.8 (q), 22.5 (q); MS m/z 233 (0.5), 202 (7.2), 174 (33), 158 (14), 75 (100); IR (CHCl3) 2915, 1729, 1130, 1065 cm-1; Anal. Calcd for C11H23NO4 (233.30): C, 56.63; H, 9.94; N, 6.00. Found: C, 57.49; H, 9.90; N, 6.24.

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

Application of 7252-83-7, A common heterocyclic compound, 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, molecular formula is C4H9BrO2, 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.

Following a modified procedure,[9] under a N2 atmosphere, 8a (867 mg, 1.44 mmol) andCs2CO3 (3.05 g, 9.36 mmol) were placed in a 100 mL sealed tube. 2-Bromo-1,1-dimethoxyethane (9) (1.60 g, 9.5 mmol) and solvent DMF (30 mL) were added via cannula.The reaction mixture was stirred at 110 C for 24 h. At ambient temperature, the mixture wasdiluted with EtOAc (250 mL) and washed with H2O (3¡Á60 mL) and brine (60 mL). Theorganic phase was dried over Na2SO4 and concentrated. The residue was purified by columnchromatography over silica gel (n-hexane/EtOAc 5/1) to give S10 (804 mg, 81%) as acolorless solid. M. p. = 162-163 C. 1H NMR (300 MHz, CDCl3) delta = 6.92 (s, 1H), 6.91 (s,1H), 6.92-6.78 (m, 4H), 6.79 (d, J = 8.8 Hz, 1H), 6.71 (d, J = 1.1 Hz, 1H), 4.85 (t, J = 5.5 Hz1H), 4.62-4.41 (m, 5H), 3.65 (s, 3H), 3.63 (s, 3H), 3.45 (s, 3H), 3.31 (s, 6H), 1.38 (d, J =6.1 Hz, 6H), 1.33 (d, J = 6.1 Hz, 6H), 1.31 (d, J = 6.1 Hz, 6H). 13C NMR (125 MHz, CDCl3)delta = 155.6 (Cq), 150.1 (Cq), 149.5 (Cq), 147.4 (Cq), 147.2 (Cq), 146.5 (Cq), 146.2 (Cq), 146.1(Cq), 144.0 (Cq), 127.7 (Cq), 127.4 (Cq), 123.8 (CH), 123.4 (CH), 122.2 (Cq), 118.5 (Cq),115.9 (CH), 115.2 (CH), 115.0 (CH), 114.6 (Cq), 114.5 (CH), 110.2 (Cq), 105.3 (CH), 104.4(CH), 103.5 (CH), 71.5 (CH), 71.5 (CH), 71.2 (CH), 55.9 (CH3), 55.8 (CH3), 55.6 (CH3), 55.3(CH3), 47.9 (CH2), 22.1 (CH3), 21.9 (CH3). IR (neat): 2975, 2931, 1703, 1517, 1463, 1257,1107, 1031, 752 cm-1. MS (ESI) m/z (relative intensity) 712 (100) [M+Na+], 690 (50)[M+H +], 658 (80). HR-MS (ESI) m/z calcd for C39H48NO10 [M+H+] 690.3273, found690.3267.

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

Reference:
Article; Mei, Ruhuai; Zhang, Shou-Kun; Ackermann, Lutz; Synlett; vol. 28; 14; (2017); p. 1715 – 1718;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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. Quality Control of 2-Bromo-1,1-dimethoxyethane

[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

7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, belongs to ethers-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Recommanded Product: 7252-83-7

To a solution of o-thiocresol (16. 89g, 136mmo1) in acetone (130ml) is added potassium carbonate (20. 5g, 148mmol) and a solution of bromoacetaldehyde dimethylacetal (19.93g, 123mmol) in acetone (20ml) and the reaction mixture is stirred at ambient temperature overnight. The solids are filtered and washed with diethyl ether. The filtrate is concentrated and dissolved into ethyl acetate, washed successively with water, 0.5 N NaOH, and 2N NaOH. The combined aqueous fractions are extracted with dichloromethane. The combined organic fractions are dried over anhydrous MgS04, filtered and concentrated to afford 1- [ (2, 2-dimethoxyethyl) thio] -2-methyl-benzene as a brown oil (23.4g, 90%) that is used without further purification.’H NMR (CDC13) : 8= 7.33 (1H, brd), 7.19-7. 08 (3H, m), 4.56 (1H, t), 3.38 (6H, s), 3.10 (2H, d), 2.42 (3H, s).

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

Reference:
Patent; ELI LILLY AND COMPANY; WO2005/92885; (2005); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem