Category: 102-52-3

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 102-52-3 as follows. SDS of cas: 102-52-3

ethyl 2-aminopyrazolo[l ,5-a]pyrimidine-3-carboxylateA mixture of ethyl 3,5-diamino-l H-pyrazole-4-carboxylate (1.0 g, 5.9 mmol), 1,1,3,3- tetramethoxypropane (2.9 mL, 18 mmol), triethylamine (2 mL, 10 mmol), and DMF (15 mL) was heated at 100 0C for 14 hrs, then a further 2 mL of 1,1,3,3-tetramethoxypropane was added. After adding the additional 1,1,3,3-tetramethoxypropane, a significant by-product was noted and heating was stopped immediately. The reaction was cooled to room temperature and the DMF was removed in vacuo. The residue was partitioned between DCM and water, then the organic layer was concentrated and the residue purified by silica chromatography, eluting with 95:5 DCM: 2M methanolic ammonia solution to afford 420 mg (35%) of ethyl 2-aminopyrazolo[l,5- a]pyrimidine-3-carboxylate. 1H NMR (500 MHz, CDCl3) delta 8.57 (dd, J = 4.3, 1.6, IH), 8.43 (dd, J = 6.7, 1.6, IH), 6.84 (dd, J = 6.7, 4.4, IH), 5.52 (s, 2H), 4.48 (q, J= 7.1, 2H), 1.45 (t, J= 7.1, 3H).

According to the analysis of related databases, 102-52-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GENENTECH, INC.; GIBBONS, Paul; HANAN, Emily; LIU, Wendy; LYSSIKATOS, Joseph P.; MAGNUSON, Steven R.; MENDONCA, Rohan; PASTOR, Richard; RAWSON, Thomas E.; SIU, Michael; ZAK, Mark E.; ZHOU, Aihe; ZHU, Bing-Yan; WO2011/3065; (2011); A2;,
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Reference of 102-52-3,Some common heterocyclic compound, 102-52-3, name is 1,1,3,3-Tetramethoxypropane, molecular formula is C7H16O4, 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.

100 mg (0.215 mmol) of Example 12 A were mixed with 1.00 mL (6.07 mmol) 1, 1,3,3- tetramethoxypropane. The reaction mixture was heated to 175C for lh using a microwave oven. The reaction mixture was treated with DCM/MeOH and one drop of triethylamine. The solvents were removed under reduced pressure. The mixture was purified by preparative HPLC (eluent A: water + 0.13 % TFA, eluent B: MeOH) yielding 45 mg (54 %) of the title compound.HPLC-MS (Method 3): R, = 1.36 minMS (ESI pos): m/z = 387 (M+H)+

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,1,3,3-Tetramethoxypropane, its application will become more common.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; HEINE, Niklas; EICKMEIER, Christian; FERRARA, Marco; GIOVANNINI, Riccardo; ROSENBROCK, Holger; SCHAENZLE, Gerhard; WO2012/20022; (2012); A1;,
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102-52-3, name is 1,1,3,3-Tetramethoxypropane, 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. category: ethers-buliding-blocks

Stage 5- Preparation of 3-(phenylamino)allylidene)aniline hydrochloride (Bioorg. Med. Chem. 2006, 4, 92-97). Compound having formula (VI) where n=1. 24.7 g of aniline in solution in 300 mL of 0.75 N HCl is added drop by drop to 21.8 g of 1,1,3,3-tetramethoxypropane in solution in 300 mL of 0.75 N HCl. The appearance of an intense orange colour and the precipitation of an orange crystalline solid are observed. The medium is then left under stirring for 3 hours at 50 C. The cooled medium is filtered, vacuum-dried to obtain 15.2 g of orange solid (Yd=44.2%). C15H14N2, HCl-(Mass ESI+400 C. MH+=223.1).

The synthetic route of 102-52-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CENTRE NATIONAL DE LA RECHERCHE SCIENTIFIQUE (CNRS); PIERRE FABRE MEDICAMENT; Guminski, Yves; Imbert, Thierry; Pesnel, Sabrina; Pillon, Arnaud; Le Pape, Alain; Lerondel, Stephanie; US2013/183247; (2013); A1;,
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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. 102-52-3, name is 1,1,3,3-Tetramethoxypropane, This compound has unique chemical properties. The synthetic route is as follows., category: ethers-buliding-blocks

Example 22; Part A:To a solution of 4-(methylsulfonyl)phenylhydrazine (5.0 g, 26.8 mmol, 1.00 equiv) and 1 ,1 ,3,3-tetramethoxypropane (4.4 ml_, 26.8, 1.0 equiv) in ethanol (37 ml_) at rt was added concentrated HCI (2.8 mL). The resulting solution was heated at reflux for 1 hr, cooled to 0 0C and filtered to give 1-(4-methanesulfonyl-phenyl)-1/-/- pyrazole as a yellow solid (4.73 g, 79%). LCMS: (MH)+ = 223.1 (1.19 min).

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 102-52-3.

Reference:
Patent; SCHERING CORPORATION; WO2008/82487; (2008); A2;,
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Adding a certain compound to certain chemical reactions, such as: 102-52-3, name is 1,1,3,3-Tetramethoxypropane, 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 102-52-3, Safety of 1,1,3,3-Tetramethoxypropane

1,1,3,3-Tetramethoxypropan (0.16 g, 1.0 mmol) was added dropwise to a stirred solution of 4-hydrazinyl-6-methyl-2-(pyridin-2-yl)pyrimidine (0.20 g, 1.0 mmol) in a mixture of water (2 ml) and concentrated HCl acid (0.4 ml) at 40 C. The reaction mixture was stirred for 1 h, cooled down, diluted with CHCl3 and washed with the saturated solution of NaHCO3, then with water, and dried over MgSO4. After CDCl3 removal under reduced pressure the residue crystallized. Yield: 0.18 g (75%), m.p. 97 C (from hexane). Anal. Calc. for C13H11N5: C, 65.77; H, 4.62; N, 29.56. Found: C, 65.82; H, 4.64; N, 29.54%. 1H NMR (CDCl3, 300.15 MHz) delta (ppm): 8.85 (ddd, 1H, J = 4.7, 1.8, 1.0 Hz, 6-Hpyridine), 8.76 (dd, 1H, J = 2.7, 0.4 Hz, 5-Hpyrazole), 8.52 (dt, 1H, J = 7.7, 1.0 Hz, 3-Hpyridine), 7.86 (dt, 1H, J = 7.7, 1.8 Hz, 4-Hpyridine), 7.79 (s, 1H, 5-Hpyrimidine), 7.80-7,78 (m, 1H, 3-Hpyrazole), 7.40 (ddd, 1H, J = 7.7, 4.7, 1.0 Hz, 5-Hpyridine), 6.51 (dd, 1H, J = 2.7, 1.6 Hz, 4-Hpyrazole), 2.72 (s, 3H, Me). IR (KBr pellet, nu cm-1): 3161w, 3130w, 3076m, 3055w, 3008w, 2918w, 1587vs, 1560vs, 1523s, 1458vs, 1441s, 1394s, 1379s, 1225m, 1149w, 1115w, 1037m, 985w, 951m, 914m, 862m, 810m, 760s, 740m, 679w, 604m, 584w.

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, 1,1,3,3-Tetramethoxypropane, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Bushuev, Mark B.; Gatilov, Yuri V.; Nikolaenkova, Elena B.; Vasiliev, Vladimir G.; Krivopalov, Viktor P.; Inorganica Chimica Acta; vol. 395; (2013); p. 95 – 103;,
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Reference of 102-52-3,Some common heterocyclic compound, 102-52-3, name is 1,1,3,3-Tetramethoxypropane, molecular formula is C7H16O4, 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 amixtureof5.0g (19.6 mmol) ofL-tryptophan methylesterand50 mLof methanol,6.0 mL(23.6 mmol) of 1,1,3,3-tetramethoxypropane wasadded. The reaction mixture wasadjusted pH 1-2 withHCl(5N) and stirred at 45 Cfor 48h. The mixture was evaporatedto dryness in vacuo, the residue wasdissolved in a mixture ofwater(30mL) and ethyl acetate (30mL),and the aqueousphasewas extracted with ethyl acetate (30mL×3). The organic phase wascombined, washed successively with 10%Na2CO3andsaturatedNaCl,dried over anhydrousNa2SO4, filtered, andevaporatedto dryness in vacuo. The residue was purified by chromatographyonsilica gel (Chloroform: Methanol, 30:1) toobtain5.4 g of the title compound as pale yellow oilin 88.5% yield.ESI-MS (m/e) 319 [M+H]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,1,3,3-Tetramethoxypropane, its application will become more common.

Reference:
Article; Wu, Jianhui; Zhao, Ming; Wang, Yuji; Wang, Yaonan; Zhu, Haimei; Zhao, Shurui; Peng, Shiqi; Bioorganic and Medicinal Chemistry Letters; vol. 26; 19; (2016); p. 4631 – 4636;,
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Ether | (C2H5)2O – PubChem

Adding a certain compound to certain chemical reactions, such as: 102-52-3, name is 1,1,3,3-Tetramethoxypropane, 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 102-52-3, Computed Properties of C7H16O4

1. The starting precursor 2-bromomalonaldehydewas prepared using procedure given in literature [S. Trofimenko, J.Org. Chem. 28(11) (1963), 3243-3245.], [W.J. Tomsho, J.J. McGuire, K. Coward, Org. Biomol. Chem. 3(18) (2005)3388-3398.].To a 100 ml of aqueous solution of 1,1,3,3-tetramethoxypropane (1) (100g, 0.12 M) added concentrated HCl (4.3 ml) and stirred untilit forms homogeneous solution, the temperature of the reaction mixturemaintained was below 35 0C,then slowly added bromine (0.15 M) solution drop wise.After the completeaddition of bromine, stirring was continued for another 30 minutes. Then thereaction mixture was concentrated under vacuum, maintaining the temperature below50 0C until thick slurry was obtained. The obtained slurry waswashed with 200 ml cold water and 100 ml of cold dichloromethane and dried invacuum. Yield: 65%, MP: 148 0C (Lit: 146-147 0C [W.J. Tomsho, J.J. McGuire, K. Coward, Org. Biomol. Chem. 3(18) (2005)3388-3398.],148 0C [M.J. Grard, Compt. Rend. Acad. Sciences. 190 (1930)187:Ann.1930, 13, 336.].

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:
Article; Yallur, Basappa Chanabasappa; Katrahalli, Umesha; Krishna, Panchangam Murali; Hadagali, Manjunatha Devagondahalli; Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy; vol. 222; (2019);,
Ether – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 102-52-3, name is 1,1,3,3-Tetramethoxypropane, 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 102-52-3, category: ethers-buliding-blocks

To a solution of ethyl 3,5-diamino-lH-pyrazole-4-carboxylate (5.00 g, 29.38 mmol) in DMF (80 mL) were added 1 , 1 ,3,3-tetramethoxypropane (14.50 mL, 88.15 mmol) and AcOH (0.34 mL, 5.88 mmol). The reaction mixture was stirred at 100 C for 14 h, and then concentrated in vacuo. The residue was partitioned between DCM (50 mL) and water (50 mL). The organic phase was separated and the aqueous phase was extracted with DCM (100 mL x 3). The combined organic phases were washed with brine (100 mL), dried over anhydrous Na2S04, filtered and concentrated in vacuo. The residue was purified by a silica gel column chromatography (a solution of NH3in MeOH (7 M)/DCM (v/v) =1/100) to give the title compound as a pale yellow solid (3.52 g, 58.1%).MS (ESI, pos. ion) m/z: 207.1 [M+H]+; H NMR (400 MHz, CDC1 ): delta (ppm) 8.60 (dd, J= 4.40 Hz, 1.76 Hz, 1H), 8.46 (dd, J = 6.76 Hz, 1.76 Hz, 1H), 6.86 (dd, J = 6.72 Hz, 4.40 Hz, 1H), 4.50 (q, J = 7.08 Hz, 2H), 1.47 (t, J = 7.08 Hz, 3H).

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, 1,1,3,3-Tetramethoxypropane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; CALITOR SCIENCES, LLC; SUNSHINE LAKE PHARMA CO., LTD.; XI, Ning; LI, Minxiong; LI, Xiaobo; WO2015/73267; (2015); A1;,
Ether – Wikipedia,
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These common heterocyclic compound, 102-52-3, name is 1,1,3,3-Tetramethoxypropane, 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. Quality Control of 1,1,3,3-Tetramethoxypropane

82.1 g (0.5 mol) of 1, 1, 3, 3-tetramethoxypropane and 39.7 g (0.45 mol) of 1,3-dimethylurea were dissolved in 400 ml of methanol, 49.0 g (0.5 mol) of concentrated sulfuric acid was added dropwise thereto at room temperature, and the mixture was allowed to undergo the reaction at 50C for 30 minutes. After completion of the reaction, this was cooled to room temperature, and the precipitated crystals were collected by filtration to obtain 59.7 g (yield 69%) of the title compound (purity 99.8%, melting point 203 – 205C).

The synthetic route of 1,1,3,3-Tetramethoxypropane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sankio Chemical Co., Ltd.; EP1559711; (2005); A1;,
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Related Products of 102-52-3, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 102-52-3 name is 1,1,3,3-Tetramethoxypropane, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

A solution of 1,1,3,3-tetramethoxypropane (23) (10 g) and concentrated HCl (0.43 mL) in H2O (11 mL) was stirred at room temperature for 10 min. Br2 (3.1 mL) was added dropwise to the solution at room temperature for more than 50 min. The reaction mixture was stirred at room temperature for 20 min and concentrated in vacuo. The residual solid was washed with H2O to give 24 (3.6 g, 39%) as a yellow solid. Mp 147-148 C; 1H NMR (CDCl3) delta 4.73-4.80 (1H, m), 8.47 (2H, br s); FAB MS m/e (M-H)- 149.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,1,3,3-Tetramethoxypropane, and friends who are interested can also refer to it.

Reference:
Article; Inoue, Takayuki; Morita, Masataka; Tojo, Takashi; Yoshihara, Kousei; Nagashima, Akira; Moritomo, Ayako; Ohkubo, Mitsuru; Miyake, Hiroshi; Bioorganic and Medicinal Chemistry; vol. 21; 5; (2013); p. 1219 – 1233;,
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