HRID1672733

反应详情

EQUATION

反应方程式

HRID 1672733 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Heat the mixture of 4-chloro-N-(4,4-difluoro-cyclohexyl)-butyramide (0.41 g, 1.7 mmol) and 0.69 g of NaH in 17 mL of THF to 70° C. for overnight. Dilute the reaction mixture with Et2O. Filter the precipitate through a pad of celite. Wash the organic layer with saturated aqueous NaCl, dry over Na2SO4, filter and concentrate. Purify the crude material by chromatography to afford 0.19 g of the title compound: mass spectrum (m/z): 204 (M+1).

WORKUP

后处理

  1. temperatureHeat
  2. filtrationFilter the precipitate through a pad of celite
  3. washWash the organic layer with saturated aqueous NaCl
  4. dry with materialdry over Na2SO4
  5. filtrationfilter
  6. concentrationconcentrate
  7. customPurify the crude material by chromatography