反应详情

To a mixture of the product of part (ii) (1.2 g, 4.2 mmole) and triethylamine (0.5 g, 5 mmole) in methylene chloride (20 ml) was added, dropwise, phenyl chloroformate (0.8 g, 5.1 mmole) and the resulting mixture was stirred at room temperature for 20 hours. The reaction was quenched by the addition of water, the aqueous phase separated and re-extracted with methylene chloride. The combined organic extracts were washed with aqueous sodium bicarbonate solution then water, dried over magnesium sulphate and concentrated under reduced pressure to provide a solid. Trituration of this solid material with ethanol yielded the desired product, m.p. 197°-198° (1.4 g, 83%), which was used without further purification.

1. additionwas added
2. customThe reaction was quenched by the addition of water
3. customthe aqueous phase separated
4. extractionre-extracted with methylene chloride
5. washThe combined organic extracts were washed with aqueous sodium bicarbonate solution
6. dry with materialwater, dried over magnesium sulphate
7. concentrationconcentrated under reduced pressure
8. customto provide a solid