反应详情

To a solution of 9.8 g (0.025 mole) of 2,7-bis(4-piperidinobutyryl)xanthene in 300 ml of glacial acetic acid is added 9.8 g (0.033 mole) of sodium dichromate over 1/2 hour. The mixture is stirred for 11/2 hours, refluxed for 1 hour, then evaporated to near dryness, cooled, diluted with water and made alkaline with 28% NH4OH solution. The resulting solid is extracted with methylene chloride, chromatographed on alumina using methylene chloride as the eluant, recrystallized from heptane and dried under vacuum at 60°C to give the title compound, M.P. 93°-95°C.

1. temperaturerefluxed for 1 hour
2. customevaporated
3. temperaturecooled
4. additiondiluted with water
5. extractionThe resulting solid is extracted with methylene chloride
6. customchromatographed on alumina
7. customrecrystallized from heptane
8. customdried under vacuum at 60°C