반응 #741222

반응 방정식

2-benzyloxy-5-fluoro-3-(trifluoromethyl)-benzoic acid ethyl ester

2-hydroxy-2-(2,2-dimethyl-1,3-dioxolan-4-yl)-ethylamine

→

2-Benzyloxy-5-fluoro-(trifluoromethyl)-benzoic acid-[2-hydroxy-2-(2,2-dimethyl-I,3-dioxolan-4-yl)-ethylamide]

용매

ethanol

반응 조건

후처리

1. 1
   workup.DISTILLATIONthe ethanol is distilled off
2. 2
   workup.DISSOLUTIONThe reaction mixture is then dissolved in 50 ml of ethyl acetate
3. 3
   기타is dried on sodium sulfate
4. 4
   농축concentrated by evaporation
5. 5
   기타the residue is chromatographed on silica gel 60 with ethyl acetate/hexane
6. 6
   기타2.18 g (7.18 mol) =47.68% of the theoretical yield
7. 7
   기타is obtained as an amorphous solid

실험 절차

3.42 g (10 mmol) of 2-benzyloxy-5-fluoro-3-(trifluoromethyl)-benzoic acid ethyl ester is dissolved in 10 ml of ethanol, 2.43 g (15 mmol) of 2-hydroxy-2-(2,2-dimethyl-1,3-dioxolan-4-yl)-ethylamine is added, the ethanol is distilled off and the remaining oil is warmed to 100° C. in a vacuum in 2 hours. The reaction mixture is then dissolved in 50 ml of ethyl acetate, shaken out twice with 10 ml of 1N hydrochloric acid each, the organic phase is dried on sodium sulfate, concentrated by evaporation and the residue is chromatographed on silica gel 60 with ethyl acetate/hexane. 2.18 g (7.18 mol) =47.68% of the theoretical yield is obtained as an amorphous solid.

출처