Acetic Acid → HCID 14402879, Verbindung

HRID 1381825Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1381825
C(O)(=O)C.O.[C:6]([CH2:8][N:9]1[C:14]2[CH:15]=[C:16]([N+:19]([O-])=O)[CH:17]=[CH:18][C:13]=2[O:12][CH2:11][C:10]1=[O:22])#[N:7]>[Fe].C(O)C>[NH2:19][C:16]1[CH:17]=[CH:18][C:13]2[O:12][CH2:11][C:10](=[O:22])[N:9]([CH2:8][C:6]#[N:7])[C:14]=2[CH:15]=1

Komponenten

6

Edukt 3

HCID 176Acetic AcidHCID 962WaterHCID 14402878HCID 14402878, Verbindung

Produkt 1

HCID 14402879HCID 14402879, VerbindungAusbeute 74,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23925IronKatalysatorHCID 702EthanolLösungsmittel2×

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A mixture of ethanol (15 ml), acetic acid (1 g), water (25 ml) and iron (3 g) is stirred at 80° C., and 4-cyanomethyl-6-nitro-2H-1,4-benzoxazin-3(4H)-one (2.33 g) is added portionwise thereto. The whole is stirred at 80° C. until gas evolution ceases. The reaction mixture is mixed with active carbon (1 g) and ethanol (20 ml), refluxed for 15 minutes, and filtered. The filtrate is poured into chilled water. The deposited crystals are collected by filtration, and dried to obtain 6-amino-4-cyanomethyl-2H-1,4-benzoxazin-3(4H)-one (1.51 g).

Aufarbeitung

  1. stirringThe whole is stirred at 80° C. until gas evolution ceases
  2. temperaturerefluxed for 15 minutes
  3. filtrationfiltered
  4. additionThe filtrate is poured
  5. temperatureinto chilled water
  6. filtrationThe deposited crystals are collected by filtration
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-715ca77a502248729df48cda7b5786db
Quelldatensatz
uspto-grants-1989_02
Patentnummer
US04804394

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