反应详情

A solution of 3,3′-thiodipropanol (900 mg, 6 mmol) in THF (3 ml) was added dropwise to a suspension of sodium hydride (240 mg, 6 mmol) in THF (15 ml) under an atmosphere of N2. The reaction mixture was stirred at RT for 30 mins, then a solution of tert-butyldimethylsilylchloride (900 mg, 6 mmol) in THF (2 ml) was added and stirring was continued for 16 hours. The reaction mixture was partitioned between EtOAc and water. The organic layer was separated, washed with brine, dried (Na2SO4) and evaporated in vacuo. The resulting residue was purified by silica gel chromatography eluting with 20% EtOAc in cyclohexane to give the title compound as a colourless oil (793 mg).

1. stirringstirring
2. waitwas continued for 16 hours
3. customThe reaction mixture was partitioned between EtOAc and water
4. customThe organic layer was separated
5. washwashed with brine
6. dry with materialdried (Na2SO4)
7. customevaporated in vacuo
8. customThe resulting residue was purified by silica gel chromatography
9. washeluting with 20% EtOAc in cyclohexane