反应 #1882379

反应方程式

2-((R)-1-Methyl-pyrrolidin-3-yloxy)-4-nitrobenzotrifluoride

hydrogen

magnesium sulfate

→

product

3-((R)-1-Methyl-pyrrolidin-3-yloxy)-4-trifluoromethyl-phenylamine

溶剂

ethyl acetate

反应条件

后处理

1. 1
   过滤then filtered through a pad of Celite
2. 2
   洗涤The filter cake was rinsed with ethyl acetate (2×25 ml)
3. 3
   其他the filtrate was evaporated under reduced pressure to an oil
4. 4
   其他This oil was evaporated twice for dichloromethane (50 ml)
5. 5
   其他to remove

实验过程

A solution of 2-((R)-1-Methyl-pyrrolidin-3-yloxy)-4-nitrobenzotrifluoride (7.8 g, 26.9 mmol) in ethyl acetate (50 ml) was treated with 10% platinum on carbon (200 mg) then subjected to 40 psi hydrogen pressure for 3 hrs. The slurry was treated with anhydrous magnesium sulfate (5 g) then filtered through a pad of Celite. The filter cake was rinsed with ethyl acetate (2×25 ml) then the filtrate was evaporated under reduced pressure to an oil. This oil was evaporated twice for dichloromethane (50 ml) to remove trapped ethyl acetate. This gave the product as a clear light brown oil that solidified on standing (6.9 g, 99%): LCMS 249 (M++H).

来源