HRID1583893

反应详情

EQUATION

反应方程式

HRID 1583893 的结构方程式

PROCEDURE

实验过程

L-aspartic acid, 13.3. parts, was added to 100 parts by volume of 2N aqueous sodium hydroxide and the resulting solution was cooled to 0°-10° C. in an ice bath. Diketene, 8.4 parts, was added and the resulting two phase mixture was stirred for 2.5 hours at 0°-10° C. The homogeneous solution was washed twice with 100 parts by volume of ether and the aqueous layer was acidified with 16.6 parts by volume of concentrated hydrochloric acid. This solution was extracted three times with 100 parts by volume of ethyl acetate, the combined extracts were dried over sodium sulfate, filtered and the solvent evaporated under vacuum at 25°-30° C. to give 2.3 parts of N-aceto-acetyl-L-aspartic acid, mp 127°-129.5° C.

WORKUP

后处理

  1. temperaturethe resulting solution was cooled to 0°-10° C. in an ice bath
  2. washThe homogeneous solution was washed twice with 100 parts by volume of ether
  3. extractionThis solution was extracted three times with 100 parts by volume of ethyl acetate
  4. dry with materialthe combined extracts were dried over sodium sulfate
  5. filtrationfiltered
  6. customthe solvent evaporated under vacuum at 25°-30° C.