反应 #710498

反应方程式

2-chloro-6-(trifluoromethyl)nicotinic acid

BH3-THF

→

[2-chloro-6-(trifluoromethyl)pyridin-3-yl]methanol

溶剂

NaHCO3

THF

反应条件

后处理

1. 1
   浓缩After 16 h the reaction mixture was concentrated under reduced pressure
2. 2
   其他to remove THF
3. 3
   其他The resulting reaction mixture
4. 4
   萃取extracted with ethyl acetate (2×500 mL)
5. 5
   洗涤The combined organic layers were washed with water (500 mL), brine (500 mL)
6. 6
   干燥dried over anhydrous sodium sulfate
7. 7
   其他the solvent was removed under reduced pressure

实验过程

To a stirred solution of e 2-chloro-6-(trifluoromethyl)nicotinic acid (Int-15) (40 g, 1.0 eq.) in THF (400 mL) was added BH3-THF (266.6 mL, 1.5 eq) at room temperature. The progress of the reaction was monitored by TLC. After 16 h the reaction mixture was concentrated under reduced pressure to remove THF. The resulting reaction mixture was diluted with 10% NaHCO3 (500 mL) and extracted with ethyl acetate (2×500 mL). The combined organic layers were washed with water (500 mL), brine (500 mL), dried over anhydrous sodium sulfate and the solvent was removed under reduced pressure to get crude [2-chloro-6-(trifluoromethyl)pyridin-3-yl]methanol (Int-16) as light yellow liquid, 32 g (85.5%).

来源