HRID446419

反应详情

EQUATION

反应方程式

HRID 446419 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of 3,3,3-trifluoropropan-1-amine hydrochloride (0.165 g) in methanol (3 mL) was added 2,2-dimethoxyacetaldehyde (60% in water, 0.17 mL) followed by sodium bicarbonate (0.093 g) and the mixture was stirred at ambient temperature overnight. A slurry of palladium on carbon 10% (50 mg) in methanol (1 mL) was added and the mixture was hydrogenated at 5 bar pressure for 4 hours. The mixture was filtered and concentrated in vacuo. The resulting gummy solid was suspended in DCM (5 mL) and dried over sodium sulphate, filtered and evaporated to give the titled compound as a yellow gum. Yield 0.152 g.

WORKUP

后处理

  1. waitthe mixture was hydrogenated at 5 bar pressure for 4 hours
  2. filtrationThe mixture was filtered
  3. concentrationconcentrated in vacuo
  4. dry with materialdried over sodium sulphate
  5. filtrationfiltered
  6. customevaporated