反应详情

温度

80 °C

Crude (4-cyano-2-hydroxymethylphenyl)(4-fluorophenyl)methanol (700 g) is dissolved in H3PO4 (60%, 3000 mL) and the solution is heated to 80° C. for 3 hours. Toluene (1000 mL) is added and the phases are separated. The aqueous phase is further extracted with toluene (1000 mL). The toluene phases are joined and the solvents are removed in vacuo. The remaining crystals are recrystallized from EtOH (99%). Yield 219 g (29%). DSC onset: 97° C.

1. customthe phases are separated
2. extractionThe aqueous phase is further extracted with toluene (1000 mL)
3. customthe solvents are removed in vacuo
4. customThe remaining crystals are recrystallized from EtOH (99%)
5. custom97° C.