HRID232884

反应详情

EQUATION

反应方程式

HRID 232884 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

0.2 g of (±)-3-buten-2-ol, 1.4 mg of palladium (II) acetate and 0.27 g of triethylamine were added to 1.36 g of 2-(7-chloro-6-fluoroquinolin-2-yl)methoxy-8-iodo-11-(2-tetrahydropyranyloxy)-6,11-dihydrodibenz[b,e]oxepine obtain in Reference example 73 dissolved in 2.5 ml of acetonitrile and the mixture was refluxed under heating for 5.5 hours. After 60 ml of methylene chloride and 60 ml of ice water were added to this reaction mixture, the organic layer was separated, washed with water and dried over anhydrous sodium sulfate. After the solvent was removed, the residue was applied to silica gel column chromatography to obtain 0.76 g of the title compound.

WORKUP

后处理

  1. customobtain in Reference example 73
  2. temperaturethe mixture was refluxed
  3. temperatureunder heating for 5.5 hours
  4. customthe organic layer was separated
  5. washwashed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. customAfter the solvent was removed