反应详情

N-(2-methoxy-5-pyridyl)-cyclopropane carboxamide (5.0 g, 0.026 mol) was added portionwise to stirred solution of phosphorus pentachloride (5.42 g, 0.026 mol) in dichloromethane (25 ml) under a nitrogen atmosphere at room temperature. After complete addition the mixture was stirred at room temperature for one hour and then heated at reflux for a further one hour. The reaction mixture was then evaporated under vacuum to give a solid product which was washed with diethyl ether (50 ml) and air dried to give N-(2-methoxy-5-pyridyl)-cyclopropylmethanimidoyl chloride as the hydrochloride salt (6.2 g, 97%) which was used in Stage 3 without further purification or characterisation.

1. additionAfter complete addition the mixture
2. temperatureheated
3. temperatureat reflux for a further one hour
4. customThe reaction mixture was then evaporated under vacuum
5. customto give a solid product which
6. washwas washed with diethyl ether (50 ml) and air
7. customdried