p-Toluohydrazide → O,O-dibutyl O-[3-(4-methylbenzoylhydrazonomethyl)phenyl] thiophosphate

HRID 1105581Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1105581
[P:1]([O:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([CH:20]=O)[CH:15]=1)([O:8][CH2:9][CH2:10][CH2:11][CH3:12])([O:3][CH2:4][CH2:5][CH2:6][CH3:7])=[S:2].[CH3:22][C:23]1[CH:32]=[CH:31][C:26]([C:27]([NH:29][NH2:30])=[O:28])=[CH:25][CH:24]=1>CO.C(Cl)Cl>[P:1]([O:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([CH:20]=[N:30][NH:29][C:27](=[O:28])[C:26]2[CH:31]=[CH:32][C:23]([CH3:22])=[CH:24][CH:25]=2)[CH:15]=1)([O:3][CH2:4][CH2:5][CH2:6][CH3:7])([O:8][CH2:9][CH2:10][CH2:11][CH3:12])=[S:2]

Komponenten

5

Edukt 2

HCID 77174p-ToluohydrazideHCID 53644866O,O-dibutyl O-(3-formylphenyl) thiophosphate

Produkt 1

HCID 54317001O,O-dibutyl O-[3-(4-methylbenzoylhydrazonomethyl)phenyl] thiophosphate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittel2×HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A solution of O,O-dibutyl O-(3-formylphenyl) thiophosphate (0.02 mole) in methanol (50 ml) and 4-methylbenzoylhydrazine (0.02 mole) are charged into a glass reaction vessel and the mixture is stirred at room temperature for a period of about 12 hours. After this time the reaction mixture is stripped of methanol under vacuum and the residue is dissolved in methylene chloride (100 ml) and the resulting solution is washed with water (75 ml), with aqueous sodium hydroxide (75 ml; 0.1 N) and again with water (75 ml). The washed solution is then dried over anhydrous magnesium sulfate, filtered and stripped of solvent to yield the desired product O,O-dibutyl O-[3-(4-methylbenzoylhydrazonomethyl)phenyl] thiophosphate.

Aufarbeitung

  1. washthe resulting solution is washed with water (75 ml), with aqueous sodium hydroxide (75 ml; 0.1 N) and again with water (75 ml)
  2. dry with materialThe washed solution is then dried over anhydrous magnesium sulfate
  3. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-7e52b3055fc4465699d936d0144338a9
Quelldatensatz
uspto-grants-1982_01
Patentnummer
US04309422

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