HRID1672103

反应详情

EQUATION

反应方程式

HRID 1672103 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

10 g (26.9 mmol) of 8-propyl-3-(3,4,5-trifluorophenyl)-7,8,9,10-tetrahydrobenzo[c]chromen-6-one from Example 1 (1.2.) are dissolved in THF and hydrogenated to cessation in the presence of palladium/active carbon catalyst. The mixture is subsequently filtered, the solvent is removed under reduced pressure, and the residue is dissolved in abs. ethanol and, after addition of 5.5 g (80.7 mmol) of sodium ethoxide, refluxed overnight. After addition of water, the mixture is acidified, the solution is extracted with MTB ether and dried over sodium sulfate. The solvent is removed under reduced pressure, and the crude product is purified by crystallisation, giving ethyl 5-propyl-2-(3′,4′,5′-trifluoro-3-hydroxybiphenyl-4-yl)cyclohexanecarboxylate.

WORKUP

后处理

  1. filtrationThe mixture is subsequently filtered
  2. customthe solvent is removed under reduced pressure
  3. dissolutionthe residue is dissolved in abs
  4. temperaturerefluxed overnight
  5. extractionthe solution is extracted with MTB ether
  6. dry with materialdried over sodium sulfate
  7. customThe solvent is removed under reduced pressure
  8. customthe crude product is purified by crystallisation