反应详情

The ketone from step 1 (0.310 g, 1.02 mmol) was dissolved in THF (3 ml), and phenyltrimethylammonium tribromide (PTT) (0.386 g, 1.02 mmol) was added as a solid leaving an orange solution which began to deposit a white solid immediately. Stirring for 1.5 hours leaves a colorless mixture to which water (5 ml) was added. THF was then evaporated and the resulting aqueous mixture was extracted with ethyl acetate. Drying over Na2SO4 and evaporation leaves a white crystalline solid (85% desired mono-brominated material by LC-MS, 5% starting material, 10% dibrominated) suitable for the next step. LC-MS (ES+): 381, 379 m/e.

1. customleaving an orange solution which
2. additionwas added
3. customTHF was then evaporated
4. extractionthe resulting aqueous mixture was extracted with ethyl acetate
5. dry with materialDrying over Na2SO4 and evaporation
6. customleaves a white crystalline solid (85% desired mono-brominated material by LC-MS, 5%