Ethanol → HCID 14347805, Verbindung

HRID 2291765Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2291765
[CH2:1]([O:3][C:4]([CH2:6][N:7]1[C:12]2[CH:13]=[CH:14][C:15]([N+:17]([O-])=O)=[CH:16][C:11]=2[O:10][CH2:9][C:8]1=[O:20])=[O:5])[CH3:2].C(O)C.[H][H]>[C].[Pd].O1CCCC1>[NH2:17][C:15]1[CH:14]=[CH:13][C:12]2[N:7]([CH2:6][C:4]([O:3][CH2:1][CH3:2])=[O:5])[C:8](=[O:20])[CH2:9][O:10][C:11]=2[CH:16]=1

Komponenten

6

Edukt 3

HCID 702EthanolHCID 111501834-ethoxycarbonylmethyl-7-nitro-2H-1,4-benzoxazin-3(4H)-oneHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 14347805HCID 14347805, VerbindungAusbeute 74,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418390HCID 178418390, VerbindungKatalysatorHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A mixture of 4-ethoxycarbonylmethyl-7-nitro-2H-1,4-benzoxazin-3(4H)-one (30 g), 10% palladium-carbon (3 g) and ethanol (150 ml) was charged in an autoclave, and catalytically reduced under conditions of 20 kg/cm2 of hydrogen pressure and at a temperature of 60° C. to 70° C. Tetrahydrofuran was added thereto, and the liquor was filtered, then the filtrate was distilled under reduced pressure. Recrystallization of the resulting solid from ethanol gave the desired 7-amino-4-ethoxycarbonylmethyl-2H-1,4-benzoxazin-3(4H)-one (20 g). mp. 136°-137° C.

Aufarbeitung

  1. additionwas charged in an autoclave
  2. filtrationthe liquor was filtered
  3. distillationthe filtrate was distilled under reduced pressure
  4. customRecrystallization of the resulting solid from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-57289f45c3b54c60a49f565a41be1a19
Quelldatensatz
uspto-grants-1989_01
Patentnummer
US04798620

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