HRID2194383
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was refluxed for 72 h
- concentrationThe reaction mixture was concentrated in vaccuo
- additionthe pH was adjusted to 7 by addition of 37% HCl solution
- extractionthe aqueous phase was extracted twice with 40 ml of ethyl acetate
- washThe organic phase was washed once with 10 of brine
- dry with materialdried with magnesium sulfate
- filtrationfiltered
- customevaporated