반응 #311573

ord-79420fbaf6684c2cb28d487ece978294

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was heated
  2. 2
    온도under reflux for 2 hrs
  3. 3
    온도, cooled
  4. 4
    여과filtered
  5. 5
    기타to remove diethylamine hydrochloride
  6. 6
    기타The filtrate was evaporated to dryness under reduced pressure
  7. 7
    기타the residue was crystallised from ethanol

실험 절차

A mixture of 2,4-bis(trichloromethyl)benzo[1,3]dioxin-6-carbonyl chloride (2 g.) and diethylamine (25 ml.) was heated under reflux for 2 hrs., cooled, and filtered to remove diethylamine hydrochloride. The filtrate was evaporated to dryness under reduced pressure, and the residue was crystallised from ethanol to give 4-dichloromethylene-N,N-diethyl-2-trichloromethylbenzo[1,3]dioxin-6-carboxamide, m.p. 123°-124° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04232032uspto-grants-1980_11