反应详情

The crude product 7 (1.0 g, 2.4 mmol) from the above reaction was dissolved in methylene chloride (10 mL), treated with anhydrous HBr gas for 1 h until disappearance of 7 on TLC. The reaction mixture was diluted with ether (100 mL) and decanted. The precipitates were washed with ether and decanted (3×100 mL). The remaining ether was removed in vacuo and the residue was dried under vacuum to afford 8 (0.88 g, 100%) as a white solid. MS m/z 366.0 (MH+), 286.1 (MH+−HBr).

1. customdecanted
2. washThe precipitates were washed with ether
3. customdecanted (3×100 mL)
4. customThe remaining ether was removed in vacuo
5. customthe residue was dried under vacuum