HRID2302130
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
69 g of hydroxylamine hydrochloride, 30.5 g of 2-hexyldecylbromide, 0.5 g of EDTA and 500 ml of methanol were mixed and thereto 84 g of sodium hydrogencarbonate was added. The resulting mixture was heated under reflux for 3 hours. Then, the reaction mixture was concentrated, ethyl acetate and water were added thereto, the solution obtained was extracted by liquid separation, and the organic phase was dried over magnesium sulfate. The dried organic phase was concentrated and bis(2-hexyldecyl)hydroxylamine as a by-product was removed using silica gel column chromatography to produce the objective compound. The product was a colorless liquid. Yield: 10.5 g (40.9%).
WORKUP
后处理
- temperatureThe resulting mixture was heated
- temperatureunder reflux for 3 hours
- concentrationThen, the reaction mixture was concentrated
- additionethyl acetate and water were added
- customthe solution obtained
- extractionwas extracted by liquid separation
- dry with materialthe organic phase was dried over magnesium sulfate
- concentrationThe dried organic phase was concentrated
- custombis(2-hexyldecyl)hydroxylamine as a by-product was removed
- customto produce the objective compound