Benzylaniline → 1-cyclopentyl-2-phenyl-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide

HRID 2058885노트

반응식

HRID 2058885 반응식
[CH2:1]([NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:15]1([P:20](Cl)(Cl)=[O:21])[CH2:19][CH2:18][CH2:17][CH2:16]1>CC1CCCCC1>[CH:15]1([P:20]2(=[O:21])[C:3]3[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=3[CH2:1][N:8]2[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH2:19][CH2:18][CH2:17][CH2:16]1

참가 물질

4

반응물 2

HCID 66028BenzylanilineHCID 15267393P-Cyclopentylphosphonic dichloride

생성물 1

HCID 130374861-cyclopentyl-2-phenyl-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide

시약·촉매·용매 1

HCID 7962Methylcyclohexane용매

실험 절차

The procedure of Example 1 was employed utilizing N-benzylaniline and cyclopentyl phosphonic dichloride. The crude product produced as a result of the chromatographic separation was slurried in methylcyclohexane and further purified on a chromatographic system employing an alumina column using chloroform (containing 0.75% ethyl alcohol) as the eluant. Fractions containing the benzazaphosphole were crystallized using benzene and methylcyclohexane to yield 1-cyclopentyl-2-phenyl-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide as a yellow solid. A second crop was obtained to give a total yield of 0.85 g (5% yield) of 1-cyclopentyl-2-phenyl-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide having a melting point of 123°-125° C. and the following analysis:

후처리

  1. customThe crude product produced as
  2. customa result of the chromatographic separation
  3. customfurther purified on a chromatographic system
  4. additionFractions containing the benzazaphosphole
  5. customwere crystallized

출처 및 근거

ORD 기록
ord-5476abfdd4bc497aa3d939192c2ef6dc
출처 데이터셋
uspto-grants-1982_03
특허 번호
US04319913

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