HRID2119587
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 mixture of 613 mg (2.9 mmol) 2-methyl phenacylbromide (literature: WO9907666), 691 mg (2.4 mmol) [3-(3-Dimethylaminomethylene-thioureido)-propyl]-carbamic acid tert-butyl ester and 1 ml (7.2 mmol) NEt3 in 20 ml ethanol was heated to 100° C. for 16 h. The mixture was concentrated and purified by flash column chromatography on silica eluting with ethyl acetate/n-hexane 1/1. The combined product fractions were evaporated and 693 mg (77%) of the title compound (MS (m/e): 375.9 (MH+, 100%)) were obtained.
WORKUP
后处理
- concentrationThe mixture was concentrated
- custompurified by flash column chromatography on silica eluting with ethyl acetate/n-hexane 1/1
- customThe combined product fractions were evaporated