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
To a suspension of 0.98 g of lithium aluminum hydride in 50 ml of dried tetrahydrofuran (THF), a solution of 3 g of N-acetylhomoveratrylamin in 25 ml of THF was added dropwise with stirring. After heating for 3 hours under reflux, the reaction mixture was cooled with ice and gradually added dropwise under violent stirring with a solvent mixture composed of 10 ml of water and 10 ml of THF. Insoluble matter was filtered off and the filtrate was concentrated. The residue obtained was dissolved in 50 ml of ethyl acetate, washed twice with water and dried over anhydrous sodium sulfate. After distilling off the solvent under reduced pressure, N-ethyl-homoveratrylamine was obtained as oily product. The yield was 2.3 g.
WORKUP
后处理
- temperatureAfter heating for 3 hours
- temperatureunder reflux
- temperaturethe reaction mixture was cooled with ice
- additiongradually added dropwise
- stirringunder violent stirring with a solvent mixture
- filtrationInsoluble matter was filtered off
- concentrationthe filtrate was concentrated
- customThe residue obtained
- washwashed twice with water
- dry with materialdried over anhydrous sodium sulfate
- distillationAfter distilling off the solvent under reduced pressure