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
- 120 °C
PROCEDURE
实验过程
Cesium fluoride (0.048 g, 0.320 mmol), palladium tetrakis(triphenylphosphine) (0.018 g, 0.016 mmol) and CuI (0.0060 g, 0.032 mmol) were added to a solution of 2-(2-amino-pyrimidin-4-yl)-3-iodo-1-methyl-4-oxo-1,4,6,7-tetrahydro-pyrrolo[3,2-c]-pyridine-5-carboxylic acid tert-butyl ester (prepared as described in Example 1) (0.075 g, 0.160 mmol) and 3-nitro-benzyl tributyl stannane (0.102 g, 0.240 mmol) in dry DMF (1.5 ml) under an argon atmosphere. The reaction mixture was stirred at 120° C. under microwave irradiation for 1 h. The reaction mixture was diluted with purite water (2.0 ml) and the precipitate was filtered, dissolved into DCM and purified on silica gel (DCM/MeOH from 100:0 up to 85:15), affording 2-(2-Amino-pyrimidin-4-yl)-1-methyl-3-(3-nitro-benzyl)-4-oxo-1,4,6,7-tetrahydro-pyrrolo[3,2-c]pyridine-5-carboxylic acid tert-butyl ester (0.0558 g, 0.116 mmol, 73%).
WORKUP
后处理
- filtrationthe precipitate was filtered
- dissolutiondissolved into DCM
- custompurified on silica gel (DCM/MeOH from 100:0 up to 85:15)