反应详情

温度

135 °C

A mixture of compound 10G (1.0 g, 3.28 mmol), (2-chloro-acetyl)-carbamic acid tert-butyl ester (1.0 g, 5.0 mmol) and Na2HPO4 (1.4 g, 10 mmol) in DMA (50 mL) was stirred at 135° C. for four hours. Solvent was removed under reduced pressure. The residue was sonicated in ethyl acetate/water, and the precipitate was filtered off. Ethyl acetate solution was separated and concentrated and loaded on silica gel. The silica column was eluted with hexane/ethyl acetate (1/2) to give 0.45 g of desired product (10H). ESI-MS:m/z 444.1 (M+H)+.

1. customSolvent was removed under reduced pressure
2. customThe residue was sonicated in ethyl acetate/water
3. filtrationthe precipitate was filtered off
4. customEthyl acetate solution was separated
5. concentrationconcentrated
6. washThe silica column was eluted with hexane/ethyl acetate (1/2)