反应详情

温度

40 °C

At 0° C., 4.1 ml (55.60 mmol) of thionyl chloride were added dropwise to 4.70 g of the compound from Example 20A in 50 ml of methanol. The mixture was stirred at 0° C. for 0.5 hours and at 40° C. overnight. After cooling, the mixture was concentrated, the residue was taken up in ethyl acetate and washed with saturated aqueous sodium bicarbonate solution, the aqueous phase was extracted repeatedly with ethyl acetate and the combined organic phases were dried over sodium sulphate, filtered and concentrated. This gave 392 mg (61% of theory from Example 16A) of the title compound as a diastereomer mixture which was reacted without further purification.

1. temperatureAfter cooling
2. concentrationthe mixture was concentrated
3. washwashed with saturated aqueous sodium bicarbonate solution
4. extractionthe aqueous phase was extracted repeatedly with ethyl acetate
5. dry with materialthe combined organic phases were dried over sodium sulphate
6. filtrationfiltered
7. concentrationconcentrated
8. customThis gave 392 mg (61% of theory from Example 16A) of the title compound as a diastereomer mixture which was reacted without further purification