反应详情

To a solution of 12 (3.08 g, 11.0 mmol) in carbon tetrachloride under Argon was added N-bromosuccinimide (1.96 g, 11.0 mmol). The contents of the reaction flask were heated to reflux. After 3 h an additional portion of N-bromosuccinimide (0.50 g, 2.81 mmol) was added to the reaction flask. After 7 h the solvent was removed in vacuo and sat. sodium bicarbonate was added. Extracted with methylene chloride (4×) and dried the combined organic portions with magnesium sulfate (anh.). Removal of the solvent in vacuo followed by trituration with ether gave 13 as a light solid (3.47 g, 9.70 mmol, 88.2%)

1. temperatureThe contents of the reaction flask were heated to reflux
2. customAfter 7 h the solvent was removed in vacuo and sat. sodium bicarbonate
3. additionwas added
4. extractionExtracted with methylene chloride (4×)
5. dry with materialdried the combined organic portions with magnesium sulfate (anh.)
6. customRemoval of the solvent in vacuo