反应详情

Sodium hydride (80% dispersion in oil; 360 mg) was suspended in dry DME (50 ml) under nitrogen and 5,6-dihydro-4-methoxy-2(1H)-pyridinone (1.27 g) in dry DME (20 ml) was added slowly. The resulting suspension was stirred at 20° for 1 h. 4-(Chloromethyl)-5-methyl-1-(triphenylmethyl)-1H-imidazole (3.72 g) in dry DME (50 ml) was added, and after the initial reaction had subsided the mixture was heated to 50° for 4 h and then cooled. Methanol (5 ml) was added dropwise, and solvent was removed invacuo. 8% Aqueous sodium bicarbonate solution (300 ml) was added to the residue and the resulting solution was extracted with dichloromethane (2×300 ml), dried and evaporated in vacuo to leave an oil which was purified by FCC eluting with System A (200:8:1) to give the title compound (2.84 g), m.p. 181°-184°.

1. customafter the initial reaction
2. temperaturewas heated to 50° for 4 h
3. temperaturecooled
4. customsolvent was removed invacuo
5. addition8% Aqueous sodium bicarbonate solution (300 ml) was added to the residue
6. extractionthe resulting solution was extracted with dichloromethane (2×300 ml)
7. customdried
8. customevaporated in vacuo
9. customto leave an oil which
10. customwas purified by FCC
11. washeluting with System A (200:8:1)