Synthetic Route of 33420-52-9, Adding some certain compound to certain chemical reactions, such as: 33420-52-9, name is 2,2-Difluoropropan-1-ol,molecular formula is C3H6F2O, 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 33420-52-9.
To a cooled (0 C) solution of 2,2-difluoropropan-l-ol (3.17 g, 33.0 mmol) and pyridine (2.97 mL, 36.7 mmol) in CH3CN (100 mL) was added dropwise Tf20 (5.70 mL, 33.8 mmol). The reaction was stirred for 30 min at 0 C. To the cooled slurry was added a cold solution of methyl 4-methyl-5-(l-(piperidin-4-yl)propyl)thiophene-3 -carboxylate hydrochloride (2.6 g, 7.34 mmol) and K2C03 (9.13 g, 66.0 mmol) in CH3CN (20 mL). The reaction was allowed to warm to RT, then heated at 50 C overnight. The reaction was evaporated to dryness under vacuum, taken up in DCM, washed with water, brine, dried (Na2S04), filtered, and concentrated under vacuum. The residue was purified by silica gel chromatography (Isco RediSep Rf Gold 120 g, 5% EtOAc:hexanes) to give methyl 5-(1- (1-(2,2-difluoropropyl)piperidin-4-yl)propyl)-4-methylthiophene-3-carboxylate (2.05 g, 5.42 mmol, 73.8 % yield) as a yellow oil. 1H NMR (400 MHz, CDCl3) delta 8.00 (s, 1H), 3.85 (s, 3H), 2.99 (d, J=11.12 Hz, 1H), 2.86 (d, J=11.12 Hz, 1H), 2.53-2.75 (m, 3H), 2.37 (s, 3H), 2.04-2.27 (m, 2H), 1.84-2.01 (m, 2H), 1.62 (t, J=18.69 Hz, 4H), 1.30-1.47 (m, 5H), 0.76 (t, J=7.33 Hz, 3H). MS(ES) [M+H]+ 360.2.
According to the analysis of related databases, 33420-52-9, the application of this compound in the production field has become more and more popular.
Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY (NO.2) LIMITED; KNIGHT, Steven David; NEWLANDER, Kenneth Allen; TIAN, Xinrong; (112 pag.)WO2016/66697; (2016); A1;,
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