HRID507686

反应详情

EQUATION

反应方程式

HRID 507686 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

5-(2-Chloroethoxy)benzo[b]thiophene (0.25 g, 1.17 mmol) was dissolved in DMF (3 mL) and treated with morpholine (0.205 mL, 2.35 mmol) and sodium iodide (0.035 g, 0.235 mmol). The mixture was heated to 70° C. and stirred overnight. The reaction was cooled down to room temperature and poured into a saturated aqueous solution of sodium bicarbonate (20 mL), which was extracted several times with ethyl acetate. All the organic extracts were combined and washed with a saturated aqueous solution of sodium bicarbonate, water and brine. The ethyl acetate layer was then dried with sodium sulfate and purified by flash chromatography using a gradient of 0 to 8% methanol in dichloromethane to obtain a clear oil. Yield=0.237 g. MS (M+H)+ 264.

WORKUP

后处理

  1. temperatureThe reaction was cooled down to room temperature
  2. extractionwas extracted several times with ethyl acetate
  3. washwashed with a saturated aqueous solution of sodium bicarbonate, water and brine
  4. dry with materialThe ethyl acetate layer was then dried with sodium sulfate
  5. custompurified by flash chromatography
  6. customto obtain a clear oil