HRID370930

反应详情

EQUATION

反应方程式

HRID 370930 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methyl 5-[(4-chlorophenyl)(methylimino)methyl]-1,4-dimethyl-1H-pyrrole-2-acetate perchlorate (1.5 g, 3.6 mmole) was dissolved in chloroform, extracted with saturated aqueous sodium bicarbonate, dried over sodium sulfate, and concentrated. The residue was treated with dimethyl sulfate (0.5 g, 3.9 mmole) and allowed to stand at 18°-30° C. for two hours. The reaction was dissolved in methanol (10 ml) and treated with saturated aqueous sodium bicarbonate (5 ml) and water (2 ml). The solution was heated at reflux overnight, then allowed to cool to room temperature. The solid was isolated by filtration, washed with water, and air dried to yield 0.95 g (76%) of the title compound as a light tan solid, m.p. >230° C.

WORKUP

后处理

  1. extractionextracted with saturated aqueous sodium bicarbonate
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated
  4. temperatureThe solution was heated
  5. temperatureat reflux overnight
  6. customThe solid was isolated by filtration
  7. washwashed with water, and air
  8. customdried