HRID414562

反应详情

EQUATION

反应方程式

HRID 414562 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 11.6 mg of cuprous iodide, 86 mg of bis (triphenylphosphine) palladium (II) dichloride, 1.5 g of 6-bromo-3,4-dihydrocarbostyril and 774 mg of N-propargylimidazole was stirred in a mixture of 10 ml of pyridine and 2 ml of triethylamine at 100° C. for 48 hours under nitrogen. The reaction was then treated with 10 ml of saturated aqueous potassium carbonate and extracted with a solution of 10% methanol in methylene chloride. The extract was dried over anhydrous sodium sulfate, the solvent removed under reduced pressure and the residue chromatographed on silica gel eluting with 4% methanol in methylene chloride, yielding 6-[3-(imidazol-1-yl)-prop-1-yn-1-yl]-3,4-dihydrocarbostyril, m.p. 164°-168° C.

WORKUP

后处理

  1. extractionextracted with a solution of 10% methanol in methylene chloride
  2. dry with materialThe extract was dried over anhydrous sodium sulfate
  3. customthe solvent removed under reduced pressure
  4. customthe residue chromatographed on silica gel eluting with 4% methanol in methylene chloride