Diethyl Ether → N'-t-butyl-N'-[methyl-(2-chlorophenylamino)phosphinyl]-N-benzoylhydrazine

HRID 1197296

Reaktionsgleichung

Reaktionsgleichung von HRID 1197296
[CH3:1][P:2](Cl)Cl.[C:5]([NH:13][NH:14][C:15]([CH3:18])([CH3:17])[CH3:16])(=[O:12])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[Cl:19][C:20]1[CH:26]=[CH:25][CH:24]=[CH:23][C:21]=1[NH2:22].CC[O:29]CC>C(N(CC)CC)C.C(Cl)Cl>[C:15]([N:14]([P:2]([CH3:1])([NH:22][C:21]1[CH:23]=[CH:24][CH:25]=[CH:26][C:20]=1[Cl:19])=[O:29])[NH:13][C:5](=[O:12])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)([CH3:18])([CH3:17])[CH3:16]

Komponenten

7

Edukt 4

HCID 3283Diethyl EtherHCID 72402-ChloroanilineHCID 61194Methyl phosphonous dichlorideHCID 299436N'-tert-butylbenzohydrazide

Produkt 1

HCID 19368069N'-t-butyl-N'-[methyl-(2-chlorophenylamino)phosphinyl]-N-benzoylhydrazine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

Methyl dichlorophosphine (1.3 g) in ether (10 ml) and triethylamine (2 ml) were added to a stirred solution of N-benzoyl-N'-t-butyl hydrazine (1.0 g) in methylene chloride (3 ml). After stirring 5 minutes at room temperature, o-chloroaniline was added neat producing a mild exotherm. The reaction was quenched 2 minutes later with water (20 ml) and ether (20 ml), separated and the organic washed with 0.1N HCl, dried over MgSO4, filtered and rotavapped to a colorless oil weighing 0.5 g.

Aufarbeitung

  1. customproducing a mild exotherm
  2. customThe reaction was quenched 2 minutes later with water (20 ml) and ether (20 ml)
  3. customseparated
  4. washthe organic washed with 0.1N HCl
  5. dry with materialdried over MgSO4
  6. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-aa5e45900ad1411a93bc0c8578495b35
Quelldatensatz
uspto-grants-1992_05
Patentnummer
US05117057

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