반응 #46893

반응 방정식

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

용매

THF

반응 조건

후처리

1. 1
   기타most of the solvent was removed under reduced pressure
2. 2
   workup.ADDITIONThe residue was mixed with 20 mL water
3. 3
   기타the resulting solid was collected
4. 4
   세척washed with water
5. 5
   기타The obtained yellow crystalline material was dried under reduced pressure at 35° C

실험 절차

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.

출처