HRID2218732

反应详情

EQUATION

反应方程式

HRID 2218732 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperaturereflux for 5 h
  2. concentrationConcentrate
  3. customthe reaction in vacuo
  4. washwash with 1N sodium hydroxide solution
  5. customSeparate the layers
  6. washwash with brine
  7. dry with materialdry over sodium sulfate
  8. filtrationPurity using filter chromatography
  9. washeluting with 10% ethyl acetate