HRID1280571

反应详情

EQUATION

反应方程式

HRID 1280571 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

[1-(2,2,2-Trifluoroethyl)piperidin-4-yl]-carbamic acid tert-butyl ester was then taken up in dioxane (80 mL) and hydrogen chloride gas was bubbled through the solution for 10 minutes. The reaction vessel was capped tightly and stirred for 1.5 hours. The solvent was removed under reduced pressure at 40° C. The residue was taken up in 42 mL of 0.5M sodium methoxide in methanol, stirred at room temperature for 3 hours, and filtered. The filtrate was concentrated, taken up in ethyl acetate, filtered, and concentrated to give 1.0 g of 1-(2,2,2-trifluoroethyl)piperidin-4-ylamine as a dark colored oil, (M+H)+=183.

WORKUP

后处理

  1. customhydrogen chloride gas was bubbled through the solution for 10 minutes
  2. customThe reaction vessel was capped tightly
  3. customThe solvent was removed under reduced pressure at 40° C
  4. stirringstirred at room temperature for 3 hours
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated
  7. filtrationfiltered
  8. concentrationconcentrated