HRID68561

反应详情

EQUATION

反应方程式

HRID 68561 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

700 mg (3-(4-fluoro-3-methyl-phenyl)-5-phenyl-pyrazol-1-yl)-acetic acid was dissolved in 10 mL DMF. 869 mg TBTU and 465 μL DIPEA were added to this solution and the mixture was stirred 1 min at RT. 448 mg 4-chloro-6-piperazine-1-yl-pyrimidine was added and stirring was continued for 2 h. Then 10 mL of a 1M NaOH solution and 50 mL CH2Cl2 were added, the organic phase was separated. The solvent was removed. The residue was dissolved in dichlormethane, water was added and the layers were separated. The organic layer was evaporated and the residue was purified by flash chromatography (silica gel, DCM/MeOH 0-30 to yield 500 mg of the desired compound.

WORKUP

后处理

  1. stirringstirring
  2. waitwas continued for 2 h
  3. customthe organic phase was separated
  4. customThe solvent was removed
  5. dissolutionThe residue was dissolved in dichlormethane
  6. additionwater was added
  7. customthe layers were separated
  8. customThe organic layer was evaporated
  9. customthe residue was purified by flash chromatography (silica gel, DCM/MeOH 0-30