HRID128042

反应详情

EQUATION

反应方程式

HRID 128042 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

233.4 g (1 mol) of 3,3-dimethyl-12-isopropyl-1-aza-1,5,9-cyclododecatriene is added dropwise to 100 g of 37% hydrochloric acid and 200 ml of water in the course of one hour, in a manner ensuring that the temperature does not exceed 80° C. The mixture is then cooled to 20°-50° C., and 69.5 g (1.0 mol) of hydroxylamine hydrochloride is added. There is subsequently added during one hour, while cooling with a water bath, about 92 g (2.3 mols) of solid sodium hydroxide until the pH value of the aqueous solution is 10-11. The organic phase which precipitates is separated, and washed free from salt with water. Distillation yields 245 g (0.92 mol) of 2,2-dimethyl-11-isopropyl-11-amino-undeca-4,8-dienal-oxime; b.p. 158°-162° C./4 Pa; nD20 =1.4930.

WORKUP

后处理

  1. customdoes not exceed 80° C
  2. temperatureThe mixture is then cooled to 20°-50° C.
  3. additionThere is subsequently added during one hour
  4. temperaturewhile cooling with a water bath
  5. customThe organic phase which precipitates
  6. customis separated
  7. washwashed free from salt with water
  8. distillationDistillation