反应详情

温度

120 °C

A stirred mixture of 0.380 g of Compound 31A, 0.50 mL of N,N-diisopropylethylamine, 0.545 g of Compound 2B and 3 mL of N,N-dimethylformamide was heated at 120° C. for 5 h. The solution was diluted with water (60 mL) and extracted with dichloromethane (3×30 mL); the organic layer was washed with water (3×20 mL), dried (anhydrous sodium sulphate) and evaporated to dryness in vacuo. The residue was purified by flash chromatography (chloroform-2N methanolic ammonia 100:1) affording 0.373 g (43.7%) of the title compound as an ivory solid. M.p. 139-141° C.

1. extractionextracted with dichloromethane (3×30 mL)
2. washthe organic layer was washed with water (3×20 mL)
3. dry with materialdried (anhydrous sodium sulphate)
4. customevaporated to dryness in vacuo
5. customThe residue was purified by flash chromatography (chloroform-2N methanolic ammonia 100:1)