HRID63288

反应详情

EQUATION

反应方程式

HRID 63288 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1,1-dimethylethyl 7-(5-fluoro-2-{[(4-methyl-2-pyridinyl)methyl]oxy}phenyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate, (0.304 g) was dissolved in a minimum amount of dioxane. The solution was cooled in ice and to this was added a solution of HCl in dioxane (2 ml). This was stirred until the reaction had gone to completion by tlc. The reaction mixture was concentrated in vacuo. The product salt was dissolved in water and backwashed with ethyl acetate. The aqueous was neutralised with aqueous sodium hydroxide (1M). This was extracted with ethyl acetate. The organics were dried over sodium sulphate and concentrated to give the title compound, 100 mg.

WORKUP

后处理

  1. temperatureThe solution was cooled in ice
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. dissolutionThe product salt was dissolved in water
  4. extractionThis was extracted with ethyl acetate
  5. dry with materialThe organics were dried over sodium sulphate
  6. concentrationconcentrated