HRID1247592

反应详情

EQUATION

反应方程式

HRID 1247592 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred suspension of tert-butyl 3-(4-{[(1-adamantylmethyl)amino]carbonyl}-5-chloropyridin-2-yl)prop-2-ynylcarbamate (Example 6(i)) (0.34 g) and 5% rhodium on carbon was stirred under a positive pressure (2 barr) of hydrogen until no further uptake was observed. The mixture was filtered and concentrated. The residue was dissolved in a solution of hydrogen chloride in 1,4-dioxane (10 ml of a 4M solution) and left to stand for 0.5 hours. The solution was concentrated and the residue triturated with ethyl acetate to afford the titled compound (0.174 g) as a beige powder.

WORKUP

后处理

  1. filtrationThe mixture was filtered
  2. concentrationconcentrated
  3. dissolutionThe residue was dissolved in a solution of hydrogen chloride in 1,4-dioxane (10 ml of a 4M solution) and
  4. waitleft
  5. concentrationThe solution was concentrated
  6. customthe residue triturated with ethyl acetate