反应 #312630

反应方程式

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

KOH

KHSO4

→

title compound

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

溶剂

EtOH

H2O

反应条件

后处理

1. 1
   萃取extracted with CHCl3
2. 2
   洗涤The organic layer washed with brine
3. 3
   干燥dried over anhydrous Na2SO4
4. 4
   浓缩concentrated under reduced pressure
5. 5
   其他The residue was purified by a silica gel column chromatography (silica gel: Wako Gel (C200), eluent: CHCl3/methanol=20:1)

实验过程

A mixture of {1-[7-(4-bromo-2,6-dimethyl-phenyl)-2,6-dimethyl-thieno[3,2-d]pyrimidin-4-yl]-piperidin-4-yl}-acetonitrile (350 mg) and KOH (492 mg) in a mixture of EtOH (1.5 mL) and H2O (1.0 mL) in a sealed tube was heated at 105° C. for 3 hours. After concentration of the reaction mixture under reduced pressure, 5% KHSO4 aqueous solution was added and extracted with CHCl3. The organic layer washed with brine, dried over anhydrous Na2SO4 and concentrated under reduced pressure. The residue was purified by a silica gel column chromatography (silica gel: Wako Gel (C200), eluent: CHCl3/methanol=20:1) to obtain the title compound (164 mg).

来源