反应详情

温度

139 °C

A mixture of 0.248 g (1 mmol)of 4-chloro-6,7-dimethoxy-quinoline-3-carbonitrile, 0.151 g (1.1 mmol) of 3-amino-2-methylbenzyl alcohol, 0.116 g (1 mmol) pyridine hydrochloride and 12 ml of 2-ethoxyethanol was heated in a 138-140° C. oil bath for 6 hours; progress of the reaction was monitored by TLC. When TLC indicated the disappearance of starting material, the reaction was cooled and concentrated in vacuo to a thick oil. To this oil was added 50 ml of water followed by 5 ml of 1M NaHCO3, approximately pH 8. The resulting precipitate was collected, washed with water and diethyl ether, and dried in vacuo at 65° C. to give 0.32 g (91.5%) of the desired product as light tan crystals. MP 123-125° C.;: mass spectrum (electrospray, m/e,): 349.9(M+H)+.

1. temperaturethe reaction was cooled
2. concentrationconcentrated in vacuo to a thick oil
3. additionTo this oil was added 50 ml of water
4. customThe resulting precipitate was collected
5. washwashed with water and diethyl ether
6. customdried in vacuo at 65° C.