HRID244275
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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
To a solution of 1,4-dihydronaphthalene (8.6 g, 86% purity, 56.8 mmol) in dichloromethane (100 mL) at 0° C., m-chloroperoxybenzoic acid (17.0 g, 77% Purity, 75.8 mmol) in dichloromethane was added. After stirring for 5 h at 0° C., the solution was filtered to separate out the precipitated m-chlorobenzoic acid. The organic layer was washed with saturated Na2CO3, water, and brine (2×50 mL each). The organic layer was dried and concentrated under reduced pressure, the residue was purified by chromatography to give compound 2 (6.1 g, 73%). 1H NMR (CDCl3): δ 3.17 (d, J=17.4 Hz, 2H), 3.31 (d, J=16.8 Hz, 2H), 3.46 (s, 2H), 7.02-7.15 (m, 4H).
WORKUP
后处理
- filtrationthe solution was filtered
- customto separate out the precipitated m-chlorobenzoic acid
- washThe organic layer was washed with saturated Na2CO3, water, and brine (2×50 mL each)
- customThe organic layer was dried
- concentrationconcentrated under reduced pressure
- customthe residue was purified by chromatography