反应 #46893

反应方程式

HCl

NaH

2,2,2-trifluoro-ethanol

2-Amino-6-fluoro-3-nitro-benzoic acid ethyl ester

→

2-Amino-3-nitro-6-(2,2,2-trifluoro-ethoxy)-benzoic acid ethyl ester

溶剂

THF

反应条件

后处理

1. 1
   其他most of the solvent was removed under reduced pressure
2. 2
   workup.ADDITIONThe residue was mixed with 20 mL water
3. 3
   其他the resulting solid was collected
4. 4
   洗涤washed with water
5. 5
   其他The obtained yellow crystalline material was dried under reduced pressure at 35° C

实验过程

420 mg NaH (60% suspension in oil) were added to a solution of 2.16 mL (29.8 mmol) 2,2,2-trifluoro-ethanol in 5 mL THF. When the gas evolution ceased, 1.0 g (4.38 mmol) 2-Amino-6-fluoro-3-nitro-benzoic acid ethyl ester was added. The resulting mixture was stirred at 0° C. for 30 minutes and at room temperature for further 30 minutes. To this mixture were added 2 mL of a 6 M aqueous HCl-solution, and most of the solvent was removed under reduced pressure. The residue was mixed with 20 mL water and the resulting solid was collected and washed with water and then hexane. The obtained yellow crystalline material was dried under reduced pressure at 35° C. Yield: 1.22 g.

来源