HRID580400

反应详情

EQUATION

反应方程式

HRID 580400 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Lithium iodide (1.08 g; 8.04 mmole) was added to 1,3,4,5-tetrahydro-3-(methoxycarbonyl)-4-(methoxyphenyl)-3-(2-propenyl)-7-(trifluoromethyl)-2H-1-benzazepin-2-one (870 mg; 2.01 mmole) in pyridine (14 ml), three drops of water were added, and the mixture was refluxed with stirring for 6.5 hours. The solution was dissolved into ethyl acetate and washed with 1N hydrochloric acid (three times). The organic layer was dried (magnesium sulfate) and concentrated giving 0.79 g of solid. The crude material was used "as is" in the next step.

WORKUP

后处理

  1. additionwere added
  2. temperaturethe mixture was refluxed
  3. washwashed with 1N hydrochloric acid (three times)
  4. dry with materialThe organic layer was dried (magnesium sulfate)
  5. concentrationconcentrated