反应详情

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

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