HRID1060844

反应详情

EQUATION

反应方程式

HRID 1060844 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Under a nitrogen atmosphere, 2-(5H-dibenzo[a,d]cyclohepten-5-yloxy)-ethanol (400 mg, 1.6 mmol), tributylphosphine (480 mg, 2.4 mmol) and 2-ethoxy-3-(4-hydroxy-phenyl)-propionic acid ethyl ester (380 mg, 1.6 mmol) were successively dissolved in dry benzene (10 mL). Solid azodicarboxylic dipiperidine (ADDP) (480 mg, 2.4 mmol) was added under stirring at 0° C. to the solution. After 10 min, the reaction mixture was brought to room temperature and the stirring was continued for 2 h. The mixture was added water and the product extracted with ethyl acetate. The combined organic phases was dried (MgSO4), and concentrated in vacuo. The residue was purified chromatography eluting with ethyl acetate/hexane (1:9) to give 350 mg (47%) of the title compound: MS 472 (M+).

WORKUP

后处理

  1. customwas brought to room temperature
  2. waitthe stirring was continued for 2 h
  3. extractionthe product extracted with ethyl acetate
  4. dry with materialThe combined organic phases was dried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified chromatography
  7. washeluting with ethyl acetate/hexane (1:9)