反应 #710488

反应方程式

sulfuric acid

N-{2-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]ethylidene}-2-(trifluoromethyl)benzamide

dichloromethane

water

→

desired product

收率 63.0%

N-{2-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]-1-methoxyethyl}-2-(trifluoromethyl)benzamide

收率 63.0%

溶剂

methanol

反应条件

后处理

1. 1
   workup.ADDITIONwas added
2. 2
   其他After separation
3. 3
   萃取the aqueous phase was extracted twice with dichloromethane
4. 4
   洗涤The combined organic phases were washed with 5 mL of water
5. 5
   干燥dried over magnesium sulfate
6. 6
   过滤filtered
7. 7
   浓缩concentrated
8. 8
   其他to yield to 0.150 g of crude material, which
9. 9
   其他was purified by chromatography on silica gel

实验过程

0.16 g of N-{2-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]ethylidene}-2-(trifluoromethyl)benzamide (Int-6) were diluted in 2 mL of methanol. 50 μL of sulfuric acid 99% were added. The reaction mixture was stirred at room temperature for 48 hours. A mixture of dichloromethane (10 mL) and water (5 mL) was added. After separation, the aqueous phase was extracted twice with dichloromethane. The combined organic phases were washed with 5 mL of water, dried over magnesium sulfate, filtered, concentrated to yield to 0.150 g of crude material, which was purified by chromatography on silica gel to yield 0.107 g (63%) of desired product N-{2-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]-1-methoxyethyl}-2-(trifluoromethyl)benzamide (Ia-111), [M+1]=427.

来源