HRID331262
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
2,3-Dihydro-1-oxo-3-phenyl-1H-inden-6-yl acetate (10.1 g, 37.9 mmol) obtained in Step 3 was placed into a flask and dissolved in CCl4 (200 mL). To the resulting solution, NBS (14.8 g, 2.2 eq) and AIBN (0.62 g, 10 mol %) were added. The resulting mixture was allowed to reflux for 1 h. Then the mixture was further irradiated by a tungsten lamp (375W) for 1.5 h. After cooling to room temperature, the precipitate was collected using a Buchner funnel. The solid was dissolved in CH2Cl2 and washed with sat. Na2S2O3, H2O, and brine. The organic layer was dried over MgSO4 and concentrated in vacuo to give the desired product (12.0 g, 92%).
WORKUP
后处理
- temperatureto reflux for 1 h
- customthe precipitate was collected
- dissolutionThe solid was dissolved in CH2Cl2
- washwashed with sat. Na2S2O3, H2O, and brine
- dry with materialThe organic layer was dried over MgSO4
- concentrationconcentrated in vacuo