HRID1820883

反应详情

EQUATION

反应方程式

HRID 1820883 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-(3,4-Dimethoxy-phenyl)-1H-pyrrolo-[2,3-b]pyridine, 1, (40 mg, 0.1 mmol) was dissolved in methylene chloride (4 mL). Aqueous potassium hydroxide (50% wt/vol, 300 μL) and tetrabutylammonium hydrogen sulfate (20 mg, 0.007 mmol) were added. The reaction mixture was stirred for 10 minutes at room temperature. Into the reaction was added 6-methyl-quinoline-8-sulfonyl chloride (68 mg, 0.28 mmol), prepared as described (Lubenets, V. I.; Stadnitskaya, N. E.; Novikov, V. P.; Russ. J. Org. Chem.; 36; 2000; 851-853) and the reaction mixture was stirred for 2 hours at room temperature. The reaction mixture was concentrated and the residue was washed with brine and ethyl acetate. The organic portion was dried with anhydrous sodium sulfate and filtered. The filtrate was concentrated and the resulting solid was washed with acetonitrile to provide 24 (43 mg, 60%). MS(ESI) [M+H+]+=460.1.

WORKUP

后处理

  1. customprepared
  2. stirringthe reaction mixture was stirred for 2 hours at room temperature
  3. concentrationThe reaction mixture was concentrated
  4. washthe residue was washed with brine and ethyl acetate
  5. dry with materialThe organic portion was dried with anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated
  8. washthe resulting solid was washed with acetonitrile