反应详情

Thionyl chloride (60 mL) is added dropwise over 30 minutes to a 0° C. solution of 2-(benzo[1,3]dioxol-5-ylmethyl-methyl-amino)-ethanol (22.2 g, 110 mmol) in DCM (250 mL) under nitrogen. The ice bath is removed, and the solution is stirred at room temperature overnight (16 h). The white slurry is concentrated under reduced pressure, diluted with brine (150 mL) and ethyl acetate (200 mL), and the precipitate is collected via vacuum filtration. The solid is washed with ethyl acetate and dried overnight under vacuum to afford 26.5 g (91%) of benzo[1,3]dioxol-5-ylmethyl-(2-chloro-ethyl)-methyl-amine hydrochloride as a white powder.

1. customThe ice bath is removed
2. concentrationThe white slurry is concentrated under reduced pressure
3. additiondiluted with brine (150 mL) and ethyl acetate (200 mL)
4. filtrationthe precipitate is collected via vacuum filtration
5. washThe solid is washed with ethyl acetate
6. customdried overnight under vacuum