HRID2370910

反应详情

EQUATION

反应方程式

HRID 2370910 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 60.1 mg (0.23 mmol) of the compound from example 1g, 37.7 mg (0.23 mmol) of bromocyclohexane and 100 μl of triethylamine in 1 ml of absolute THF was treated in a microwave at 170° C. for 40 min. The reaction solution was then taken up in a little EA/water (1:1), and the phases were separated off, dried over Na2SO4, filtered and evaporated to dryness. Purification by chromatography on RP silica gel with CH3CN/water/0.1% TFA as mobile phase and freeze-drying of the combined product fractions afforded 18.0 mg of the desired compound as bistrifluoroacetate in the form of an amorphous solid.

WORKUP

后处理

  1. customthe phases were separated off
  2. dry with materialdried over Na2SO4
  3. filtrationfiltered
  4. customevaporated to dryness
  5. customPurification by chromatography on RP silica gel with CH3CN/water/0.1% TFA as mobile phase
  6. customfreeze-drying of the combined product fractions