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
- 60 °C
PROCEDURE
实验过程
To a solution of {(R)-2-[5-(2-chloro-acetylamino)-3-(2,6-difluoro-benzyl)-2,6-dioxo-3,6-dihydro-2H-pyrimidin-1-yl]-1-phenyl-ethyl}-carbamic acid tert-butyl ester (44 mg, 0.08 mmol) in acetonitrile (2 mL) were added triethylamine(30 μl, 0.22 mmol) and 2-amino-ethanol (60 μl, 0.96 mmol) in that order. The solution was stirred at 60° C. for 4 hrs, cooled to room temperature, and washed with an aqueous saturated sodium bicarbonate solution to separate an organic layer. The organic layer was concentrated, and the residue was purified using silica gel chromatography (eluent: dichloromethane/methanol, 10/1) and dried in a vacuum to afford 37 mg of the compound as a colorless oil (yield 80%).
WORKUP
后处理
- temperaturecooled to room temperature
- washwashed with an aqueous saturated sodium bicarbonate solution
- customto separate an organic layer
- concentrationThe organic layer was concentrated
- customthe residue was purified
- customdried in a vacuum