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 was added 9.8 g (0.033 mole) of sodium dichromate over 1/2 hour. The mixture was 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 was 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 desired product. M.P. 93°-95°C.

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