反应 #312628

反应方程式

sodium hydrogencarbonate

7-(4-bromo-2,6-dimethyl-phenyl)-4-chloro-2,6-dimethyl-thieno[3,2-d]pyrimidine

piperidin-4-ylmethanol

N,N-diisopropylethylamine

→

{1-[7-(4-bromo-2,6-dimethyl-phenyl)-2,6-dimethyl-thieno[3,2-d]pyrimidin-4-yl]-piperidin-4-yl}-methanol

收率 94.2%

溶剂

ethanol

反应条件

后处理

1. 1
   温度was heated
2. 2
   温度at reflux for 1 day
3. 3
   萃取extracted with EtOAc
4. 4
   洗涤The organic layer washed with brine
5. 5
   干燥dried over anhydrous sodium sulfate
6. 6
   过滤filtered
7. 7
   浓缩The filtrate was concentrated under reduced pressure
8. 8
   其他purified by a silica gel column chromatography (silica gel: Wako Gel (C200), eluent: hexane/EtOAc=3:1)

实验过程

A mixture of 7-(4-bromo-2,6-dimethyl-phenyl)-4-chloro-2,6-dimethyl-thieno[3,2-d]pyrimidine (500 mg), piperidin-4-ylmethanol (226 mg), N,N-diisopropylethylamine (253 mg) in ethanol (1.5 mL) was heated at reflux for 1 day. The reaction mixture was cooled to room temperature, poured into a saturated aqueous sodium hydrogencarbonate, and then extracted with EtOAc. The organic layer washed with brine, dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated under reduced pressure and purified by a silica gel column chromatography (silica gel: Wako Gel (C200), eluent: hexane/EtOAc=3:1) to obtain {1-[7-(4-bromo-2,6-dimethyl-phenyl)-2,6-dimethyl-thieno[3,2-d]pyrimidin-4-yl]-piperidin-4-yl}-methanol as a white solid (568 mg).

来源