HRID1712335

反应详情

EQUATION

反应方程式

HRID 1712335 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The mixture of 1.08 g of 1-(3-methoxypropyl)-3,3,6-trimethyl-1,3-dihydroindol-2-one, 0.801 g of N-bromosuccinimide, 0.014 g of 2,2′-azobis(2-methylpropionitrile) and 0.021 g of dibenzoyl peroxide in 50 ml of carbon tetrachloride is heated to reflux with stirring. The reaction mixture is stirred at reflux over 1 hour (succinimide crystallizes out) and subsequently cooled to room temperature. The succinimide is filtered off and the filtrate is concentrated by evaporation. The title compound is obtained as a slightly orange oil from the residue by means of flash chromatography (SiO2 60F). Rf=0.40 (dichloromethane-diethyl ether); Rt=17.22 (II).

WORKUP

后处理

  1. temperatureis heated
  2. temperatureto reflux
  3. stirringThe reaction mixture is stirred
  4. customcrystallizes out) and
  5. filtrationThe succinimide is filtered off
  6. concentrationthe filtrate is concentrated by evaporation