HRID54103

反应详情

EQUATION

反应方程式

HRID 54103 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5 g of 3-(2-naphthyl)-L-alanine and 0.93 g of sodium hydroxide in 12 ml of water were cooled to 0° C. and stirred while a solution of 1.4 g of sodium hydroxide in 9 ml of water and 5 ml of benzyl chloroformate were added simultaneously during 10 minutes. Stirring was continued for 2 hours and the mixture was allowed to come to room temperature. The mixture was diluted with water and then extracted with diethyl ether. The aqueous layer was acidified with 4 ml of concentrated hydrochloric acid and extracted with ethyl acetate. The ethyl acetate extracts were back-washed with water. The combined ethyl acetate extracts were dried over sodium sulphate, filtered, evaporated and triturated with petroleum ether (boiling point 40°-60° C.) to give 7.5 g of N-(benzyloxycarbonyl)-3-(2-naphthyl)-L-alanine of melting point 109°-111° C.

WORKUP

后处理

  1. additionwere added simultaneously during 10 minutes
  2. customto come to room temperature
  3. extractionextracted with diethyl ether
  4. extractionextracted with ethyl acetate
  5. washThe ethyl acetate extracts were back-washed with water
  6. dry with materialThe combined ethyl acetate extracts were dried over sodium sulphate
  7. filtrationfiltered
  8. customevaporated
  9. customtriturated with petroleum ether (boiling point 40°-60° C.)