HRID2194383

反应详情

EQUATION

反应方程式

HRID 2194383 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-chloro-4-[4-(3-chloro-phenylethynyl)-2-methyl-imidazol-1-yl]-pyridine (120 mg, 0.366 mmol) was dissolved in 6 ml tert-butanol. A 50% solution of KOH (2 ml, 26.7 mmol) was added and the mixture was refluxed for 72 h. The reaction mixture was concentrated in vaccuo, the pH was adjusted to 7 by addition of 37% HCl solution, and the aqueous phase was extracted twice with 40 ml of ethyl acetate. The organic phase was washed once with 10 of brine, dried with magnesium sulfate, filtered and evaporated. The title compound (104 mg, 0.336 mmol, 92%) was obtained as a crystalline light yellow solid, MS: m/e=310.1, 312.2 (M+H+).

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 72 h
  2. concentrationThe reaction mixture was concentrated in vaccuo
  3. additionthe pH was adjusted to 7 by addition of 37% HCl solution
  4. extractionthe aqueous phase was extracted twice with 40 ml of ethyl acetate
  5. washThe organic phase was washed once with 10 of brine
  6. dry with materialdried with magnesium sulfate
  7. filtrationfiltered
  8. customevaporated