反应 #6035

ord-9eff2be66d41411fafc7473e558a11ff

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONwas added to the mixture
  2. 2
    workup.STIRRINGthe mixture was stirred at room temperature for 2 hours
  3. 3
    萃取the mixture was extracted with ethyl acetate
  4. 4
    其他dried
  5. 5
    其他condensed under reduced pressure
  6. 6
    其他purified by silica gel chromatography

实验过程

To a tetrahydrofuran solution containing 1.78 g (6.6 mmole) of 2-(4-chlorophenyl)-5-phenylvaleronitrile was added a tetrahydrofuran solution containing 0.77 g (6.9 mmole) of potassium tert-butoxide at 0° C. After stirring for 30 minutes, a tetrahydrofuran solution containing 0.5 g (6.8 mmol) of methyl isothiocyanate was added to the mixture and the mixture was stirred at room temperature for 2 hours. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate, dried and condensed under reduced pressure, and then purified by silica gel chromatography to obtain 1.19 g (yield: 52.4 %) of N-methyl-2-(4-chlorophenyl)-2-cyano-5-phenylthiovaleroamide as a crystal.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05246958uspto-grants-1993_09