反应详情

In a 500 ml round-bottom flask was mixed {[tert-butyl(diphenyl)silyl]oxy}acetic acid (17 g, 54.0 mmoles, 1 eq), thionyl chloride (11.7 g, 0.162 moles, 3 eq) and dry CH2Cl2 (120 ml, 0.45M). This mixture was refluxed for 5 hours. After cooling to room temperature the volatiles were removed in vacuo. The resulting residue was washed twice with toluene and the toluene was subsequently removed in vacuo to remove excess thionyl chloride. This resulted in 18 g (100%) of titled compound.

1. temperatureThis mixture was refluxed for 5 hours
2. customwere removed in vacuo
3. washThe resulting residue was washed twice with toluene
4. customthe toluene was subsequently removed in vacuo
5. customto remove excess thionyl chloride