反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThis compound is prepared
- additionThis solution is added dropwise under an argon atmosphere to a mixture
- temperaturecooled
- waitthe mixture is left
- customto rise to RT
- stirringAfter stirring for 1 hour at RT
- customthe THF is evaporated off under vacuum
- customThe precipitate formed
- filtrationis spin-filtered off
- washis washed with iso ether