HRID1775324

反应详情

EQUATION

反应方程式

HRID 1775324 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The product from the previous step (tert-butyl 4-(4-methylpyrimidin-2-yl)piperazine-1-carboxylate) was dissolved in a one-to-one mixture of trifluoroacetic acid and DCM (8 ml) and stirred at room temperature for three hours. The volatiles were removed under reduced pressure, the residue was dissolved in DCM and evaporated. The residue was dissolved in THF (10 ml), HCl in dioxane (4N, 2 ml) was added and the resulting precipitate was collected by repeated centrifugation, dekantation and washing with THF to yield 107 mg of a solid (0.30 mmol, 71%). MS (APCI) m/z=179.1 [M+1]+.

WORKUP

后处理

  1. customThe volatiles were removed under reduced pressure
  2. dissolutionthe residue was dissolved in DCM
  3. customevaporated
  4. dissolutionThe residue was dissolved in THF (10 ml)
  5. additionHCl in dioxane (4N, 2 ml) was added
  6. customthe resulting precipitate was collected
  7. washwashing with THF