HRID1881517

反应详情

EQUATION

反应方程式

HRID 1881517 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 4-(2,2-dimethylpropyl)-2-{2-[4-(5-fluoropyridin-2-yl)phenyl]-1-methylethyl}-N,N-dimethyl-1H-imidazole-1-sulfonamide in 1.5 N hydrochloric acid (1 mL) and THF (1 mL) was heated at 70° C. in a sealed tube overnight. The reaction mixture was basified with 10% aqueous sodium hydroxide and extracted with ethyl acetate. The combined organic extracts were dried (sodium sulfate) and concentrated in vacuo. Purification of the resulting crude product by silica preparatory plate chromatography eluting with 10% methanol/ethyl acetate afforded the title compound. LCMS: (M+H) found 352.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe combined organic extracts were dried (sodium sulfate)
  3. concentrationconcentrated in vacuo
  4. customPurification of the resulting crude product by silica preparatory plate chromatography
  5. washeluting with 10% methanol/ethyl acetate