HRID1986976
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
PROCEDURE
实验过程
After dissolving phenyl N-(2-chloro-4-hydroxyphenyl)carbamate in N,N-dimethylformamide (100 mL), cyclopropylamine (22.7 mL) was added while cooling on ice, and the mixture was stirring at room temperature overnight. Water (400 mL), ethyl acetate (300 mL) and 6N-HCl (55 mL) were then added, the mixture was stirred, and the organic layer was separated. The organic layer was washed twice with a 10% aqueous solution of sodium chloride (200 mL), and dried over magnesium sulfate. Prism crystals obtained by concentrating the solvent were filtered and washed with heptane to give 22.8 g of the titled compound (77% yield from 4-amino-3-chlorophenol).
WORKUP
后处理
- additionwas added
- temperaturewhile cooling on ice
- stirringthe mixture was stirred
- customthe organic layer was separated
- washThe organic layer was washed twice with a 10% aqueous solution of sodium chloride (200 mL)
- dry with materialdried over magnesium sulfate
- customPrism crystals obtained
- concentrationby concentrating the solvent
- filtrationwere filtered
- washwashed with heptane