反应详情

温度

45 °C

Intermediate 14a (908 mg, 6.60 mmol) was dissolved in DCM (50 mL) and N-bromosuccinimide (1.29 g, 7.26 mmol) added. The reaction was heated to 45° C. for 4 h, then cooled and partitioned between DCM (150 mL) and saturated aqueous NaHCO3 (150 mL), and extracted into DCM (3×). The combined organic layers were washed with brine, dried (MgSO4) and evaporated in vacuo. Purification by FCC, using 0-5% [2M NH3 in MeOH] in DCM, gave the title compound (900 mg, 63%). LCMS (Method 1): Rt 1.94 min, m/z 216/218 [MH+].

1. temperaturecooled
2. custompartitioned between DCM (150 mL) and saturated aqueous NaHCO3 (150 mL)
3. extractionextracted into DCM (3×)
4. washThe combined organic layers were washed with brine
5. dry with materialdried (MgSO4)
6. customevaporated in vacuo
7. customPurification by FCC