HRID1746657
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 160 °C
PROCEDURE
实验过程
A solution of 6-chloro-N-(2-methylphenyl)pyrimidine-4-carboxamide (Intermediate 18; 3.00 g; 12.11 mmol) in EtOH (30 ml) was treated with DIEA (4.17 ml; 24.2 mmol) and cyclohexyl-cyclopropanemethyl-amine (Chembridge; 3.71 g; 24.2 mmol) and heated at 160° C. for 1 h. At the end of addition the reaction mixture was concentrated in vacuo, diluted with water and extracted with EtOAc. The combined organic layers were washed with NH4Cl, NaHCO3 and brine, dried on magnesium sulfate and evaporated in vacuo to afford the title compound as a brown solid, which was purified by precipitation from cyclohexane to afford the title compound as a beige solid.
WORKUP
后处理
- additionAt the end of addition the reaction mixture
- concentrationwas concentrated in vacuo
- additiondiluted with water
- extractionextracted with EtOAc
- washThe combined organic layers were washed with NH4Cl, NaHCO3 and brine
- customdried on magnesium sulfate
- customevaporated in vacuo