HRID32734
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
- 127.5 °C
PROCEDURE
实验过程
A mixture of 4.26 mmol 2-chloro-5-methanesulfonyl-benzoic acid (see example K, step1), 0.39 mmol Copper powder and 10 ml ammonium hydroxide 25% was heated at 125-130° C. with stirring for 18 hours. Mixture was cooled to room temperature and filtered. The solid was washed with methanol. The filtrate was concentrated in vacuo. The residue was acidified with HCl 1N to pH=2. The obtained solid was washed with water and dried (HV, 50° C., 1 hour) to yield the title compound. MS (m/e): 214.1 (M−H, 100%)
WORKUP
后处理
- temperatureMixture was cooled to room temperature
- filtrationfiltered
- washThe solid was washed with methanol
- concentrationThe filtrate was concentrated in vacuo
- washThe obtained solid was washed with water
- customdried (HV, 50° C., 1 hour)