HRID419752

反应详情

EQUATION

反应方程式

HRID 419752 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add 4-[4-(4-Fluoro-3-trifluoromethyl-phenyl)-1H-imidazol-2-yl]-piperidine-1-carboxylic acid tert-butyl ester (16.03 g; 1.00 equiv; 38.77 mmoles) in 40 mL of dimethyl sulfoxide to a solution of potassium hydroxide (1.5 equiv; 58.16 mmoles; 3.26 g) in 200 mL of dimethyl sulfoxide. After 5 min at room temperature, add methyl iodide (1.1 equiv; 42.65 mmoles; 2.66 mL) in one portion. Stir at room temperature for two hours, then pour the mixture into ice water. Filter the solid, wash with water, and dry under reduced pressure. Triturate the solid in hot heptane, filter and dried under reduced pressure to give 4-[4-(4-Fluoro-3-trifluoromethyl-phenyl)-1-methyl-1H-imidazol-2-yl]-piperidine-1-carboxylic acid tert-butyl ester (8.7 g; 52.49% yield) as a white solid.

WORKUP

后处理

  1. filtrationFilter the solid
  2. washwash with water
  3. customdry under reduced pressure
  4. customTriturate the solid in hot heptane
  5. filtrationfilter
  6. customdried under reduced pressure