HRID1374137

反应详情

EQUATION

反应方程式

HRID 1374137 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A 1-litre pressure autoclave was initial charged with 4.50 g of Raney cobalt (doped with 0.3% iron) in a mixture of 285 of conc. ammonia/methanol (m/m=1.9:1) The autoclave was closed and flushed twice with 40 bar of nitrogen and then pressurized with 45 bar of hydrogen, and the mixture was then heated to 100° C. This was followed by metering in a solution of 30.0 g (0.135 mol) of (S)-2-(cyanoacetylamino)-3-(1H-imidazol-4-yl)propionic acid (prepared according to Example 3) in a mixture of 285 g of conc. ammonia/methanol (m/m=1.9:1) over the course of one hour. After further reaction at 100° C. for one hour, the reaction mixture was cooled to room temperature. The autoclave was depressurized and the catalyst was filtered off. An in-process HPLC analysis showed that the reddish-brow-n reaction solution (310.5 g) contained 9.57% (m/m) carnosine, corresponding to a selectivity of 97% for complete conversion.

WORKUP

后处理

  1. customwas closed
  2. customflushed twice with 40 bar of nitrogen
  3. customAfter further reaction at 100° C. for one hour
  4. temperaturethe reaction mixture was cooled to room temperature
  5. filtrationthe catalyst was filtered off