反应详情

To a solution of 8.0 g. (35.2 mMol) 3-(2-benzylaminoethyl)-phenol and 100 ml. ethanol there are added 35.2 mMol sodium methylate in the form of a methanolic solution and thereafter 6.8 g. (35.2 mMol) diethyl chloromalonate. After stirring for 4 hours, the reaction mixture is evaporated. 50 ml. Diethyl ether are added to the residue, as well as ice-cold 1N aqueous sodium hydroxide solution, shaken up and the ethereal phase is separated off. After drying over anhydrous sodium sulphate, the sulphate is precipitated from it by the dropwise addition of concentrated sulphuric acid, which is filtered off with suction and washed with diethyl ether. The product is very hygroscopic and is obtained in the form of a somewhat greasy mass. Yield 11.7 g. (74% of theory).

1. customthe reaction mixture is evaporated
2. additionDiethyl ether are added to the residue
3. stirringas well as ice-cold 1N aqueous sodium hydroxide solution, shaken up
4. customthe ethereal phase is separated off
5. dry with materialAfter drying over anhydrous sodium sulphate
6. customthe sulphate is precipitated from it by the dropwise addition of concentrated sulphuric acid, which
7. filtrationis filtered off with suction
8. washwashed with diethyl ether
9. customis obtained in the form of a somewhat greasy mass