反应详情

15 g (40 mmol) of 3-benzylamino-6-(3-cyclopentyloxy-4-methoxyphenyl)pyridazine are heated to reflux in a mixture of 100 ml of glacial acetic acid, 6.5 ml of concentrated hydrochloric acid, 9.8 g (0.12 mol) of cyclohexene and 3 spatula tips of Pd/C (10 percent) for 4 hours. 9.8 g of cyclohexene and Pd/C are added once again, and boiling is continued for 16 hours. The catalyst is filtered off, the solution is diluted with 1 l of water and neutralized with concentrated ammonia, and the resulting precipitate is filtered off with suction. The product is purified by chromatography on silica gel with dichloromethane. 4.8 g (42.1%) of 3-amino-6-(3-cyclopentyloxy-4-methoxyphenyl)pyridazine of m.p. 207° C. are obtained.

1. filtrationThe catalyst is filtered off
2. additionthe solution is diluted with 1 l of water and neutralized with concentrated ammonia
3. filtrationthe resulting precipitate is filtered off with suction
4. customThe product is purified by chromatography on silica gel with dichloromethane