反应详情

Dissolve 512 mg (2 mmole) of 3-hydroxymethyldibenzo[b,f]thiepin 5-oxide in 50 ml of methylene chloride and add 648 mg (3 mmole) of pyridinium chlorochromate. Stir at room temperature for 1.5 hours and then filter the mix through a bed of Florisil. Wash the Florisil with dichloromethane; and to the combined filtrate add 4 g of silica gel. Evaporate the suspension to dryness, and place the solid on top of a column of 50 g of silica and elute the title compound with a 1:9 mixture of ethyl acetate and toluene. The compound has a m.p. of 188°-190° C.

1. filtrationfilter the
2. additionmix through a bed of Florisil
3. washWash the Florisil with dichloromethane
4. additionand to the combined filtrate add 4 g of silica gel
5. customEvaporate the suspension to dryness
6. washelute the title compound
7. additionwith a 1:9 mixture of ethyl acetate and toluene