反应 #94253

ord-56644a8e2ed447a2bd7865e896f8b370

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONAfter the addition
  2. 2
    其他to rise to 20°±1° C
  3. 3
    过滤The reaction mixture was then filtered
  4. 4
    其他to remove the amine hydrochloride
  5. 5
    洗涤the organic phase washed with 10% aqueous Tartaric acid solution and water to neutrality

实验过程

To a solution of (97%) 1,3-dimethyl-3(t-butylperoxy)butyl chloroformate 5.2 g. (0.02 mole) in diethyl ether, cooled to 0°±1° C was added a solution of dimethylamine, 1.8 g. (0.04 mole) in diethyl ether over a period of 10 minutes. After the addition was complete the mixture was allowed to stir for two hours while the reaction temperature was allowed to rise to 20°±1° C. The reaction mixture was then filtered to remove the amine hydrochloride and the organic phase washed with 10% aqueous Tartaric acid solution and water to neutrality.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04129700uspto-grants-1978_12