HRID1756071

反应详情

EQUATION

反应方程式

HRID 1756071 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2,3-dimethyl-6-methylthiopyrrolo[2,3-b]pyridine (100 mg, 0.5 mmol) and phenacyl chloride (804 mg, 5 mmol) in 3 ml CH3CN was refluxed for 72 h. The solvent was evaporated and the residue chromatographed (silica, CH2Cl2 /MeOH;59/5). Pure fractions were pooled, evaporated, and taken up in 100 ml CH2Cl2. The organic layer was washed with 25 ml 2M HCl, dried over MgSO4, and evaporated leaving 64 mg (35%) pure product as the hydrochloride.

WORKUP

后处理

  1. temperaturewas refluxed for 72 h
  2. customThe solvent was evaporated
  3. customthe residue chromatographed (silica, CH2Cl2 /MeOH;59/5)
  4. customevaporated
  5. washThe organic layer was washed with 25 ml 2M HCl
  6. dry with materialdried over MgSO4
  7. customevaporated