HRID1797002

反应详情

EQUATION

反应方程式

HRID 1797002 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

C-{4-[4-(3-trifluoromethyl-phenyl)-1H-imidazole-2-yl]-cyclohexyl}-methylamine (326 mg, 1.0 mmol, from Example 1C) and TEA (102 mg, 1.0 mmol) were dissolved in CH2Cl2/THF (1:1) and brought to 0° C. with an ice bath. Acetyl chloride (79 mg, 1.0 mmol) was added to the reaction mixture slowly and the ice bath was removed. After 2 hours, the solution was diluted with CH2Cl2, added to a separatory funnel and washed with 10% NaOH (3×). The solution was dried (Na2SO4), concentrated under reduced pressure, and the residue purified using flash chromatography (5%→10% MeOH/CH2Cl2) to give (N-{4-[4-(3-Trifluoromethyl-phenyl)-1H-imidazol-2-yl]-cyclohexylmethyl}-acetamide.

WORKUP

后处理

  1. custombrought to 0° C. with an ice bath
  2. customthe ice bath was removed
  3. additionthe solution was diluted with CH2Cl2
  4. additionadded to a separatory funnel
  5. washwashed with 10% NaOH (3×)
  6. dry with materialThe solution was dried (Na2SO4)
  7. concentrationconcentrated under reduced pressure
  8. customthe residue purified