반응 #2146063

ord-102d0eb286ef45129efb098902c86bd7

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The crude product produced as
  2. 2
    기타a result of the chromatographic separation
  3. 3
    기타was crystallized from methylcyclohexane
  4. 4
    기타to yield a tan precipitate
  5. 5
    기타The tan precipitate was recrystallized from toluene and petroleum ether

실험 절차

The procedure of Example 1 was employed utilizing N-(3-trifluoromethylphenyl)-N-benzylamine and isopropyl phosphonic dichloride. The crude product produced as a result of the chromatographic separation was crystallized from methylcyclohexane to yield a tan precipitate. The tan precipitate was recrystallized from toluene and petroleum ether to yield 1-isopropyl-2-(3-trifluoromethylphenyl)-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide as beige plates. A second crop was obtained to give a total yield of 5.9 g, (29% yield) of 1-isopropyl-2-(3-trifluoromethylphenyl)-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide having a melting point of 117°-119° C. and the following analysis:

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04319913uspto-grants-1982_03