HRID1037034
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 6-methyl-1H-spiro[benzo[c][1,2]oxaborole-3,1′-cyclopentan]-1-ol (1.2 g, 6.0 mmol) in CCl4 (10 mL) under nitrogen was added NBS (1.07 g, 6.0 mmol) and BPO (145 mg, 0.6 mmol). The mixture was heated at reflux for 2 h under the light from a Sun lamp, and then it was cooled to rt, washed with aqueous NaHCO3 and brine, dried over Na2SO4 and concentrated under vacuum. The residue was purified on column chromatography to provide the product (1.2 g, yield 71.7%).
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureat reflux for 2 h under the light from a Sun lamp
- washwashed with aqueous NaHCO3 and brine
- dry with materialdried over Na2SO4
- concentrationconcentrated under vacuum
- customThe residue was purified on column chromatography