N-Methylbenzylamine → 1-phenyl-2-methyl-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide

HRID 2058915

Reaktionsgleichung

Reaktionsgleichung von HRID 2058915
[CH3:1][NH:2][CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[C:10]1([P:16](Cl)(Cl)=[O:17])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>CCOCC>[C:10]1([P:16]2(=[O:17])[C:5]3[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=3[CH2:3][N:2]2[CH3:1])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

Komponenten

4

Edukt 2

HCID 7669N-MethylbenzylamineHCID 69990Phenylphosphonic dichloride2×

Produkt 1

HCID 130375151-phenyl-2-methyl-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

The procedure of Example 36 was employed utilizing N-methyl-N-benzylamine and phenyl phosphonic dichloride. The reaction of the dilithio compound and the phenyl phosphonic dichloride was conducted at -60° C. The residue produced as a result of the distillation process was slurried in ether to yield 1-phenyl-2-methyl-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide as a white solid. A second crop was obtained and the combined product yield was recrystallized from carbon tetrachloride and petroleum ether to yield 1-phenyl-2-methyl-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide (2.25 g, 15% yield) having a melting point of 129°-130° C. and the following analysis:

Aufarbeitung

  1. customwas conducted at -60° C
  2. customThe residue produced as
  3. customa result of the distillation process

Quellen und Nachweise

ORD-Eintrag
ord-5985f867f1654ca4ad48ab272a6f89db
Quelldatensatz
uspto-grants-1982_03
Patentnummer
US04319913

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