反应详情

Tris-(8-chlorocarbonyl-2,2,6,6-tetramethyl-benzo[1,2-d:5,4-d']-bis(1,3)oxathiol-4-yl)methanol (0.80 g, 0.80 mmol) was dissolved in benzene (200 mL). A solution of of bis(2-hydroxyethyl)amine (8.0 g, 48 mmol) in water (200 mL) was added and after vigorous stirring overnight, the mixture was transferred to a separatory funnel. The aqueous layer was removed and the remaining solid plus the benzene layer was evaporated, dissolved in methanol and passed through a short column (neutral alumina). After elution of unwanted materials with acetonitrile, the amide was eluted with methanol. After evaporation, the product was stirred with water (50 mL) at 40° C. for 2 h and then isolated by filtration. After drying, 0.60 g (60%) of the pure amide was obtained.

1. customthe mixture was transferred to a separatory funnel
2. customThe aqueous layer was removed
3. customthe remaining solid plus the benzene layer was evaporated
4. dissolutiondissolved in methanol
5. washAfter elution of unwanted materials with acetonitrile
6. washthe amide was eluted with methanol
7. customAfter evaporation
8. stirringthe product was stirred with water (50 mL) at 40° C. for 2 h
9. customisolated by filtration
10. customAfter drying