反应详情

A slurry of 22 (21.6 g, 0.132 mol) in CHCl3 (300 ml) was treated dropwise over 15 minutes with 2-(bromoacetyl)-thiophene (10.84, 0.0476 mol, 92% pure) in CHCl3 (55 ml). The reaction mixture was stirred at room temperature for 24 hours, and then filtered to remove 10.2 g of the hydrobromide of 22. The mother liquors were concentrated to a semisolid which was swirled with 75 ml of methylene chloride and refrigerated overnight. The resultant gray solid was washed with CH2Cl2 and dried to give 10.2 grams (79%) of 23; m.p. 110°-114°. The analytical sample was dried in vacuo at 85°, m.p. 115°-117°.

1. filtrationfiltered
2. customto remove 10.2 g of the hydrobromide of 22
3. concentrationThe mother liquors were concentrated to a semisolid which
4. customwas swirled with 75 ml of methylene chloride and refrigerated overnight
5. washThe resultant gray solid was washed with CH2Cl2
6. customdried