反应详情

A mixture of N-ethyl-5-chloro-2-(cyclopropylmethoxy)benzylamine (reference example 20) (4.4 g, 18.4 mmol), 6-chloropyridazine-3-carboxamide (3.0 g 19 mmol), di-isopropylethylamine (5.0 ml, 29 mmol) and DMF (25 ml) was stirred at reflux for 16 hours. The mixture was cooled and diluted with water (50 ml), the gum was allowed to settle out and the supernatant liquor decanted. The gum was dissolved in dichloromethane and stirred while adding 2N hydrochloric acid (50 ml). A precipitate formed after 10 minutes. The solid was filtered off and washed with dichloromethane (10 ml) and ether (20 ml) to give a buff solid (3.8 g, 61%) m.p. 177-8° C.

1. temperatureat reflux for 16 hours
2. temperatureThe mixture was cooled
3. customthe supernatant liquor decanted
4. dissolutionThe gum was dissolved in dichloromethane
5. stirringstirred
6. additionwhile adding 2N hydrochloric acid (50 ml)
7. customA precipitate formed after 10 minutes
8. filtrationThe solid was filtered off
9. washwashed with dichloromethane (10 ml) and ether (20 ml)