反应详情

The product of Step B (0.120 g; 0.253 mmol) and acetoxyacetyl chloride (0.11 mL; 1.01 mmol) were added to 2 mL of acetonitrile and stirred at room temperature. After 50 minutes the reaction mixture was diluted with ethyl acetate and washed two times with aqueous sodium bicarbonate. The organic layer was dried over sodium sulfate then concentrated. The residue was triturated in 10 mL of methanol. The solid product was collected and rinsed two times with methanol then dried in vacuo. HPLC/MS 576.8 (M+2); Rt=4.32 min.

1. washwashed two times with aqueous sodium bicarbonate
2. dry with materialThe organic layer was dried over sodium sulfate
3. concentrationthen concentrated
4. customThe residue was triturated in 10 mL of methanol
5. customThe solid product was collected
6. washrinsed two times with methanol
7. customthen dried in vacuo