반응 #50577

ord-6f5869ef032345849333c43b75a8a347

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONare added in portions
  2. 2
    온도with cooling
  3. 3
    workup.STIRRINGthe mixture is stirred for 2 hours at room temperature and for a further 5 hours
  4. 4
    온도at reflux temperature
  5. 5
    여과The entire batch is then filtered while hot and
  6. 6
    농축concentrated in vacuo

실험 절차

15.0 g (83.8 mmol) of 2,3-dichloro-thiophenol are introduced into 50 ml of absolute methanol, 4.5 g (83.8 mmol) of sodium methanolate are added in portions, with cooling, and the mixture is stirred for 15 minutes at room temperature. 6.3 g (83.8 mmol) of chloroacetonitrile are subsequently added dropwise, and the mixture is stirred for 2 hours at room temperature and for a further 5 hours at reflux temperature. The entire batch is then filtered while hot and concentrated in vacuo. 10.8 g (59.1% of theory) of 2,3-dichloro-phenylthioacetonitrile are obtained.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05428047uspto-grants-1995_06