反应 #1435760

反应方程式

Water

triethylamine

2-chloro-3-methyl-6-pyridin-4-yl-3H-pyrimidin-4-one hydrochloride

(1S)-2,5-diaza-bicyclo[2.2.1]heptane-2-carboxylic acid tert-butyl ester

→

pure product

收率 72.1%

(1S)-5-(1-Methyl-6-oxo-4-pyridin-4-yl-1,6-dihydro-pyrimidin-2-yl)-2,5-diaza-bicyclo[2.2.1]heptane-2-carboxylic acid tert-butyl ester

收率 72.1%

溶剂

dimethylformamide

反应条件

后处理

1. 1
   萃取the resulting solution extracted with ethyl acetate
2. 2
   洗涤The combined extracts are washed with saturated aqueous ammonium chloride and saturated aqueous sodium chloride
3. 3
   其他then-evaporated
4. 4
   温度The crude product is refluxed in diethylether for 1 h

实验过程

A mixture containing 10.7 ml (78.14 mmol) of triethylamine, 13.6 g (52.7 mmol) of 2-chloro-3-methyl-6-pyridin-4-yl-3H-pyrimidin-4-one hydrochloride (1:1), 6.0 g (30.24 mmol) of (1S)-2,5-diaza-bicyclo[2.2.1]heptane-2-carboxylic acid tert-butyl ester in 500 ml of anhydrous dimethylformamide is stirred at 20° C. for 6 h. Water is added to the cooled mixture and the resulting solution extracted with ethyl acetate. The combined extracts are washed with saturated aqueous ammonium chloride and saturated aqueous sodium chloride then-evaporated. The crude product is refluxed in diethylether for 1 h to afford 8.36 g of pure product as a brown solid.

来源