HRID1619078

反应详情

EQUATION

反应方程式

HRID 1619078 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1-(1H-Pyrrol-2-yl)-ethanone (0.980 g, 8.98 mmol) in dichloromethane (10 mL), anhydrous aluminum trichloride (3.05 g, 22.9 mmol) were added and the suspension was vigorously stirred for 15 minutes. Trichloro-acetyl chloride (1.53 mL, 13.74 mmol) in 7 mL of dichloromethane was slowly added and the mixture was then refluxed for 3 hours. The reaction mixture was cooled and poured into an iced solution of 75 mL of HCl 2N and vigorously stirred for 2 hours. Organic layer was separated and then washed with a saturated solution of NaHCO3 (2×100 mL) and water (80 mL), dried over sodium sulfate, filtered, and concentered in vacuo to give 1.061 g of (46%) of the title compound as a pale brown solid.

WORKUP

后处理

  1. temperaturethe mixture was then refluxed for 3 hours
  2. temperatureThe reaction mixture was cooled
  3. stirringvigorously stirred for 2 hours
  4. customOrganic layer was separated
  5. washwashed with a saturated solution of NaHCO3 (2×100 mL) and water (80 mL)
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered