反应详情

A mixture of 3-amino-4,4-difluoro-7-methoxy-1-heptene (420 mg, 2.3 mmoles) and N-carbetoxyphthalimide (506 mg, 2.3 mmoles) in benzene (9 ml) is kept at 25° C. overnight. After concentration under reduced pressure, the residue is dissolved in dichloromethane (5 ml) and treated with triethylamine (0.7 ml) for 41/2 hours. After addition of dichloromethane, the solution is washed with 1N HCl and water. Usual work-up affords an oil (610 mg) which is purified by chromatography on silica (ethyl acetate/petroleum ether: 20/80 RF: 0.4): 440 mg (62%).

1. concentrationAfter concentration under reduced pressure
2. dissolutionthe residue is dissolved in dichloromethane (5 ml)
3. additiontreated with triethylamine (0.7 ml) for 41/2 hours
4. additionAfter addition of dichloromethane
5. washthe solution is washed with 1N HCl and water