HRID2370910
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customthe phases were separated off
- dry with materialdried over Na2SO4
- filtrationfiltered
- customevaporated to dryness
- customPurification by chromatography on RP silica gel with CH3CN/water/0.1% TFA as mobile phase
- customfreeze-drying of the combined product fractions