HRID31342

反应详情

EQUATION

反应方程式

HRID 31342 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

This compound is prepared according to the procedure disclosed in WO 95/18105. A solution of 2-methoxyphenylmagnesium bromide is prepared from 16 g of magnesium in 35 ml of ether and from a solution of 124 g of 1-bromo-2-methoxybenzene in 175 ml of ether. This solution is added dropwise under an argon atmosphere to a mixture, cooled beforehand in an ice bath, of 30 g of 5-chloro-1H-indole-2,3-dione in 250 ml of THF and then the mixture is left stirring while allowing the temperature to rise to RT. After stirring for 1 hour at RT, the reaction mixture is slowly poured into saturated NH4Cl solution and the THF is evaporated off under vacuum. The precipitate formed is spin-filtered off and is washed with iso ether. 42 g of the expected product are obtained, which product is used without further purification in the following stage.

WORKUP

后处理

  1. customThis compound is prepared
  2. additionThis solution is added dropwise under an argon atmosphere to a mixture
  3. temperaturecooled
  4. waitthe mixture is left
  5. customto rise to RT
  6. stirringAfter stirring for 1 hour at RT
  7. customthe THF is evaporated off under vacuum
  8. customThe precipitate formed
  9. filtrationis spin-filtered off
  10. washis washed with iso ether