Water → N,N'-bis(phthalimido)oxamide N-methyl-2-pyrrolidone

HRID 1447748

Reaktionsgleichung

Reaktionsgleichung von HRID 1447748
[C:1]1(=[O:11])[O:6][C:4](=[O:5])[C:3]2=[CH:7][CH:8]=[CH:9][CH:10]=[C:2]12.[C:12]([NH:18][NH2:19])(=[O:17])[C:13]([NH:15][NH2:16])=[O:14].[CH3:20][N:21]1[CH2:25][CH2:24][CH2:23][C:22]1=[O:26].[OH2:27]>C1(C)C=CC=CC=1>[C:22]1(=[O:26])[N:16]([NH:15][C:13]([C:12]([NH:18][N:19]2[C:1](=[O:11])[C:2]3=[CH:10][CH:9]=[CH:8][CH:7]=[C:3]3[C:4]2=[O:5])=[O:17])=[O:14])[C:9](=[O:27])[C:10]2=[CH:2][CH:1]=[CH:25][CH:24]=[C:23]12.[CH3:20][N:21]1[CH2:9][CH2:10][CH2:2][C:1]1=[O:6]

Komponenten

6

Edukt 4

HCID 962WaterHCID 6811Phthalic AnhydrideHCID 13387N-methyl-2-pyrrolidoneHCID 13826Oxalic acid, dihydrazide

Produkt 1

HCID 70604243N,N'-bis(phthalimido)oxamide N-methyl-2-pyrrolidone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

Two moles of phthalic anhydride (296 g.) and one mole of oxalic dihydrazide (118 g.) in 500 ml. N-methyl-2-pyrrolidone and 500 ml. toluene were heated at reflux until two moles of water were removed (about two hours). The mixture was diluted with benzene and filtered. After washing with benzene, the white product was dried to constant weight at 50° C. giving an essentially quantitative yield of N,N'-bis(phthalimido)oxamide-N-methyl-2-pyrrolidone 1:2 complex.

Aufarbeitung

  1. customwere removed (about two hours)
  2. additionThe mixture was diluted with benzene
  3. filtrationfiltered
  4. washAfter washing with benzene
  5. customthe white product was dried to constant weight at 50° C.

Quellen und Nachweise

ORD-Eintrag
ord-526c9df1962348b5a18969ed43d1a994
Quelldatensatz
uspto-grants-1979_12
Patentnummer
US04178280

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