HRID36697
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
18.4 g (0.1 mol) of ethyl N-(but-2-enyl)-N-(2-oxoethyl)-carbamate are dissolved in 100 ml of dioxane, and 9 g of anhydrous sodium acetate and 9 g (0.108 mol) of N-methylhydroxylamine hydrochloride in 10 ml of water are added. The mixture is heated under reflux overnight and cooled and the salts are filtered off with suction and washed with dioxane. The filtrate is concentrated, the residue is taken up in 100 ml of water and K2CO3 is added. The mixture is extracted with CHCl3, the extract is dried over K2CO3 and concentrated and the residue is distilled.
WORKUP
后处理
- temperatureThe mixture is heated
- temperatureunder reflux overnight
- temperaturecooled
- filtrationthe salts are filtered off with suction
- washwashed with dioxane
- concentrationThe filtrate is concentrated
- additionK2CO3 is added
- extractionThe mixture is extracted with CHCl3
- dry with materialthe extract is dried over K2CO3
- concentrationconcentrated
- distillationthe residue is distilled