反应 #312631

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 hydrochloride

NaOH

NaHCO3

→

title compound

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

溶剂

H2SO4

反应条件

后处理

1. 1
   workup.ADDITIONAfter addition of ice
2. 2
   萃取The mixture was extracted with EtOAc
3. 3
   洗涤the organic layer washed with brine
4. 4
   干燥dried over anhydrous Na2SO4
5. 5
   浓缩concentrated under reduced pressure
6. 6
   其他The residue was purified by a silica gel column chromatography (silica gel: Wako Gel (C200), eluent: EtOAc)

实验过程

{1-[7-(4-Bromo-2,6-dimethyl-phenyl)-2,6-dimethyl-thieno[3,2-d]pyrimidin-4-yl]-piperidin-4-yl}-acetonitrile hydrochloride (30 mg) was dissolved in c H2SO4 (0.5 mL) and the solution was stirred at room temperature for 20 hours. After addition of ice, the reaction mixture was made to alkaline (pH 7) with an aqueous NaOH solution and an aqueous NaHCO3 solution. The mixture was extracted with EtOAc and 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: EtOAc) to obtain the title compound (20 mg) as a white crystal.

来源