HRID2184794

反应详情

EQUATION

反应方程式

HRID 2184794 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of β-dimethylamino-1-(2-thienyl)-2-propen-1-one (1) (18.1 g, 100 mmol) and hydroxylamine hydrochloride (7.0 g, 101 mmol) in anhydrous methanol (100 mL) is refluxed under nitrogen for 2 hrs. The reaction mixture is cooled, concentrated and partitioned between water and dichloromethane. The dichloromethane layer is dried with anhydrous sodium sulfate, filtered and concentrated to yield product (2) as a dark yellow-orange oil (14.7 g, 97 mmol, 97%).

WORKUP

后处理

  1. temperatureis refluxed under nitrogen for 2 hrs
  2. temperatureThe reaction mixture is cooled
  3. concentrationconcentrated
  4. custompartitioned between water and dichloromethane
  5. dry with materialThe dichloromethane layer is dried with anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated