反应详情

To a solution of iii (551 g, 1.78 mol) in THF (11 L) was added SnCl2.2H2O (2.17 kg, 9.62 mol) at RT. The mixture was refluxed for 3 h. The mixture was cooled to 0-5° C. and basified with saturated NaHCO3 solution and extracted with EtOAc (4×5 L). The combined organic layer were washed with brine, dried (Na2SO4), filtered and concentration in vacuo gave iv (480 g, 97%).

1. temperatureThe mixture was refluxed for 3 h
2. extractionextracted with EtOAc (4×5 L)
3. washThe combined organic layer were washed with brine
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentration in vacuo