反应 #2458203

反应方程式

triethyl amine

tert-butyl (6,7-dihydro-4H-thieno[3,2-c]pyran-4-yl)methylcarbamate

NIS

AcOH

→

desired product

tert-butyl (2-iodo-6,7-dihydro-4H-thieno[3,2-c]pyran-4-yl)methylcarbamate

溶剂

CHCl3

反应条件

后处理

1. 1
   浓缩concentrated
2. 2
   workup.ADDITIONdiluted with water
3. 3
   萃取The mixture was extracted with n-hexane
4. 4
   干燥The organic phase was dried over Na2SO4
5. 5
   浓缩concentrated
6. 6
   其他purified by column chromatography

实验过程

A solution of tert-butyl (6,7-dihydro-4H-thieno[3,2-c]pyran-4-yl)methylcarbamate (2.9 g, 1.3 mmol, 1 eq), NIS (5.2 g, 2.2 mmol, 2 eq), and AcOH (3 mL) in CHCl3 (50 mL) was stirred at room temperature for 7 hr. The reaction mixture was neutralized with triethyl amine, concentrated, and diluted with water. The mixture was extracted with n-hexane. The organic phase was dried over Na2SO4, concentrated, and purified by column chromatography to give the desired product (3 g).

来源