反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 130 °C
PROCEDURE
实验过程
1.5 g (7.15 mmol) of (±)-4-(2-chloroethyl)-3,4-dihydro-2(1H)-quinolinone are mixed intimately with 3.65 g (15 mmol) of 1-(7-methoxy-1-naphthyl)piperazine and the mixture is heated to 130° C. for 1 h while stirring. The cooled residue is taken up between 25 ml of 2N sodium hydroxide and twice 50 ml of dichloromethane. The organic extract is washed with water, dried over magnesium sulphate and concentrated. The residue is purified by elution with a dichloromethane/methanol (95:5) mixture on a silica column. The purified fraction is crystallized in ether and this solid is drained and dried. 2.6 g (87.5%) of (±)-4-{2-[4-(7-methoxy-1-naphthyl)-1-piperazinyl]ethyl}-3,4-dihydro-2(1H)-quinolinone, melting point 177°-178° C., are obtained.
WORKUP
后处理
- extractionThe organic extract
- washis washed with water
- dry with materialdried over magnesium sulphate
- concentrationconcentrated
- customThe residue is purified by elution with a dichloromethane/methanol (95:5) mixture on a silica column
- customThe purified fraction is crystallized in ether
- customdried