HRID1513948

反应详情

EQUATION

反应方程式

HRID 1513948 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dissolve 6-(2,4-difluoro-phenyl)-5-{hydroxy-[4-(2-piperidin-1-yl-ethoxy)-phenyl]-methyl}-naphthalen-2-ol (3.4 g, 7.0 mmol) in dry DMF (70 mL). Slowly add sodium hydride (440 mg, 18 mmol) and plunge into a 140° C. oil bath for 30 minutes. Cool to room temperature and pour into water. Adjust the pH to 7 and extract three times with methylene chloride. Wash combined organic layers with water, dry with sodium sulfate, filter and concentrate. Triturate with ether to yield 2.2 g (69%) of the title compound: mass spectrum (ion spray) m/z=470.3 (M+H).

WORKUP

后处理

  1. extractionextract three times with methylene chloride
  2. washWash
  3. dry with materialdry with sodium sulfate
  4. filtrationfilter
  5. concentrationconcentrate
  6. customTriturate with ether