HRID1890768

反应详情

EQUATION

反应方程式

HRID 1890768 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add K2CO3 (503 mg, 3.60 mmol) to a solution of ethyl 3-(trifluoromethyl)-1H-pyrazole-4-carboxylate (500 mg, 2.40 mmol) in acetone (8 mL) at ambient temperature under N2. Add 1-bromomethyl-4-methoxybenzene (0.51 mL, 3.6 mmol) dropwise to the mixture, and stir overnight under N2. Quench the reaction with H2O, and extract twice with EtOAc. Dry the combined organic layers over MgSO4, filter, and concentrate under reduced pressure. Purify the residue by flash silica gel chromatography (gradient of 0 to 15% EtOAc in hexanes) to yield the title compound (789 mg, quantitative). ES/MS m/z 351.0 (M+Na).

WORKUP

后处理

  1. customQuench
  2. customthe reaction with H2O
  3. extractionextract twice with EtOAc
  4. dry with materialDry the combined organic layers over MgSO4
  5. filtrationfilter
  6. concentrationconcentrate under reduced pressure
  7. customPurify the residue by flash silica gel chromatography (gradient of 0 to 15% EtOAc in hexanes)