反应详情

温度

-10 °C

Compound 3a (4.57 g, 11.92 mmol) was suspended in dry dimethoxyethane (100 mL) and cooled to −10° C. POCl3 (3.4 mL, 36.1 mmol) was added and a mixture of triethylamine (8.3 mL, 59.5 mmol) in dimethoxyethane (10 mL) was dropped slowly to the reaction mixture. After stirring for 2 h at −5° C., the reaction mixture was poured into ice water. The aqueous phase was extracted with ethyl acetate, the organic phase was washed with saturated aqueous NaHCO3 and brine, dried over Na2SO4, filtered and concentrated in vacuum. Upon refrigeration (4° C.) over night a yellow solid crystallized, which was collected and dried in vacuum.

1. additionwas dropped slowly to the reaction mixture
2. extractionThe aqueous phase was extracted with ethyl acetate
3. washthe organic phase was washed with saturated aqueous NaHCO3 and brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuum
7. customUpon refrigeration (4° C.) over night a yellow solid crystallized
8. customwhich was collected
9. customdried in vacuum