反应详情

1-Acetyl-6-bromo-5-[(1,2,3,5,6,8a-hexahydroindolizin-7-yl)methoxy]indoline (D3) (0.118 g, 0.3 mmol) and α,α'-azoisobutyronitrile (0.04 g) were stirred at reflux under Ar in benzene (40 ml) as tributyltin hydride (0.24 ml, 0.9 mmol) was added dropwise in benzene (10 ml) over 10 min. The mixture was stirred at reflux for 6 h, cooled, and extracted with dil. HCl. The extract was basified with saturated K2CO3, and extracted with chloroform. The organic extract was dried (Na2SO4) and evaporated to give the title compound (0.073 g, 77%) as a brown gum. NMR showed a mixture of two isomers.

1. temperatureat reflux for 6 h
2. temperaturecooled
3. extractionextracted with dil. HCl
4. extractionextracted with chloroform
5. extractionThe organic extract
6. dry with materialwas dried (Na2SO4)
7. customevaporated