反应详情

A mixture of (2,3-dihydro-benzo[1,4]dioxin-6-yl)methanol (10.6 g) in SOCl2 (10 mL) was stirred at room temperature for 10 min and then poured into ice-water. The organic layer was separated and the aqueous phase was extracted with dichloromethane (50 mL×3). The combined organic layers were washed with NaHCO3 (sat solution), water and brine, dried over Na2SO4 and concentrated to dryness to obtain 6-chloromethyl-2,3-dihydro-benzo[1,4]dioxine (12 g, 88% over two steps), which was used directly in next step.

1. customThe organic layer was separated
2. extractionthe aqueous phase was extracted with dichloromethane (50 mL×3)
3. washThe combined organic layers were washed with NaHCO3 (sat solution), water and brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated to dryness