반응 #1241674

반응 방정식

6-(trifluoromethyl)-isatoic acid anhydride

L-proline

→

(S)-1,2,3,11a-tetrahydro-6-(trifluoromethyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine-5,11(10H)-dione

용매

dimethyl sulphoxide

반응 조건

후처리

1. 1
   기타the solvent is removed in a high vacuum
2. 2
   기타the oil obtained
3. 3
   온도is heated to 170° for 15 minutes
4. 4
   기타The crude product is purified by chromatography on silica gel
5. 5
   세척for the elution
6. 6
   기타After recrystallization of the crude product from ethyl acetate/diethyl ether there

실험 절차

11.55 g (0.05 mol) of 6-(trifluoromethyl)-isatoic acid anhydride and 5.75 g (0.05 mol) of L-proline in 100 ml of dimethyl sulphoxide are heated to 70° for 1 hour, the solvent is removed in a high vacuum and the oil obtained is heated to 170° for 15 minutes. The crude product is purified by chromatography on silica gel using methylene chloride and mixtures of methylene chloride and ethyl acetate (5%, 10%, 15%) for the elution. After recrystallization of the crude product from ethyl acetate/diethyl ether there is obtained pure (S)-1,2,3,11a-tetrahydro-6-(trifluoromethyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine-5,11(10H)-dione of melting point 176-178°.

출처