HRID2218732
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
Dissolve 11-(3-Nitro-benzylidene-6,11-dihydro-dibenzo[b,e]oxepine (200 mg) in ethanol (10 mL) add tin chloride dihydrate (680 mg) and reflux for 5 h. Concentrate the reaction in vacuo, re-dissolve in ethyl acetate and wash with 1N sodium hydroxide solution. Separate the layers wash with brine and dry over sodium sulfate. Purity using filter chromatography eluting with 10% ethyl acetate:toluene to give 60 mg of product (56% yield).
WORKUP
后处理
- temperaturereflux for 5 h
- concentrationConcentrate
- customthe reaction in vacuo
- washwash with 1N sodium hydroxide solution
- customSeparate the layers
- washwash with brine
- dry with materialdry over sodium sulfate
- filtrationPurity using filter chromatography
- washeluting with 10% ethyl acetate