反应详情

7.54 ml of Kiliani solution (30.2 mmol of 0) was added over 6 minutes to a solution of 8.80 g (26.2 mmol) of 5-chloro-2-(2-chlorophenyl)-7-(3-hydroxybutyl)-benzoxazole in 90 ml of acetone at −5° to 0° C. After 2.5 hours, 5 ml of methanol and 50 ml of water was added. The acetone was removed in vacuo, the solid suspended, collected, washed with 0.1 N sulfuric acid until colorless and water and dried to give 8.68 g of crude product, which was dissolved in 35 ml of dichloromethane and filtered through 260 g of silica gel. A first fraction of 100 mg was discarded then 5.94 g were recovered and crystallized from di-isopropyl ether to give 5.76 g (65.8%) of title compound, mp 109-10° C.

1. customThe acetone was removed in vacuo
2. customcollected
3. washwashed with 0.1 N sulfuric acid until colorless and water
4. customdried
5. customto give 8.68 g of crude product, which
6. filtrationfiltered through 260 g of silica gel
7. custom5.94 g were recovered
8. customcrystallized from di-isopropyl ether