HRID2302130

反应详情

EQUATION

反应方程式

HRID 2302130 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe resulting mixture was heated
  2. temperatureunder reflux for 3 hours
  3. concentrationThen, the reaction mixture was concentrated
  4. additionethyl acetate and water were added
  5. customthe solution obtained
  6. extractionwas extracted by liquid separation
  7. dry with materialthe organic phase was dried over magnesium sulfate
  8. concentrationThe dried organic phase was concentrated
  9. custombis(2-hexyldecyl)hydroxylamine as a by-product was removed
  10. customto produce the objective compound