HRID430622

反应详情

EQUATION

反应方程式

HRID 430622 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

2-Amino-3-benzoyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridine (2 mmol), as prepared in Example 8, and methyl iodide (3 mmol) were dissolved in dry dimethyformamide (20 mL). Finely ground anhydrous potassium carbonate (1.9 g) and sodium iodide (0.2 g) were added to the solution and the resulting mixture was warmed to 65° C. overnight under nitrogen. After this period (TLC control), the reaction mixture was cooled, diluted with water, extracted with diethyl ether (3×50 mL), and dried on sodium sulfate. The crude product was isolated and then purified by column chromatography eluting with ethyl acetate and petroleum ether solutions to give the desired compound. (m.p. 164-165° C.; 77% yield).

WORKUP

后处理

  1. waitAfter this period (TLC control)
  2. temperaturethe reaction mixture was cooled
  3. extractionextracted with diethyl ether (3×50 mL)
  4. customdried on sodium sulfate
  5. customThe crude product was isolated
  6. custompurified by column chromatography
  7. washeluting with ethyl acetate and petroleum ether solutions