反应详情

温度

100 °C

A dried pressure tube was charged with a dispersion of (RS)-3-(3-bromo-phenyl)-5-methoxy-3-methyl-3,6-dihydro-2H[1,4]oxazine (3.91 g, 14 mmol) and ammonium chloride (4.42 g, 83 mmol) in methanol (140 ml). The tube was sealed and heated at 100° C. overnight. After cooling, the reaction mixture was evaporated to dryness. The crude product was purified on an Isolute flash NH2 column using a gradient of dichloromethane/methanol=100/0 to 75/25 as the eluent. The (RS)-5-(3-bromo-phenyl)-5-methyl-5,6-dihydro-2H-[1,4]oxazin-3-ylamine was obtained as a light yellow foam (2.71 g, 73% of theory). MS (ISP): m/z=269.2 [M+H]+, 271.1 [M+2+H]+.

1. customThe tube was sealed
2. temperatureAfter cooling
3. customthe reaction mixture was evaporated to dryness
4. customThe crude product was purified on an Isolute flash NH2 column