反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customwas closed
- customflushed twice with 40 bar of nitrogen
- customAfter further reaction at 100° C. for one hour
- temperaturethe reaction mixture was cooled to room temperature
- filtrationthe catalyst was filtered off