HRID557485
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 stirred overnight at room temperature. 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 10% brine (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 title 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 10% brine (200 mL)
- dry with materialdried over magnesium sulfate
- customPrism crystals obtained
- concentrationby concentrating the solvent
- filtrationwere filtered
- washwashed with heptane