反应详情

A mixture of 3,3-dimethylpiperidine (10 g) and triethylamine (12.3 ml) in dry dichloromethane (50 ml) was added dropwise to an ice-cold solution of bromoacetyl bromide (7.7 ml) in dry dichloromethane (100 ml). The mixture was stirred at 23° for 18 h then recooled to 0°. Iced water (200 ml) was added and the layers separated. The aqueous layer was further extracted with dichloromethane (2×200 ml) then the combined extracts were washed with 2N HCl (200 ml) and saturated brine (200 ml), dried and evaporated to give the title compound (17.28 g) as a brown oil.

1. customthen recooled to 0°
2. customthe layers separated
3. extractionThe aqueous layer was further extracted with dichloromethane (2×200 ml)
4. washthe combined extracts were washed with 2N HCl (200 ml) and saturated brine (200 ml)
5. customdried
6. customevaporated