Acetic Acid → Acetamide, N-(2-methoxy-5-nitrophenyl)-

HRID 273936

Reaktionsgleichung

Reaktionsgleichung von HRID 273936
[NH2:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[O:11][CH3:12].[C:13](O)(=[O:15])[CH3:14].C(OC(=O)C)(=O)C>O>[C:13]([NH:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[O:11][CH3:12])(=[O:15])[CH3:14]

Komponenten

5

Edukt 3

HCID 176Acetic AcidHCID 74472-Methoxy-5-nitroanilineHCID 7918Acetic Anhydride

Produkt 1

HCID 97239Acetamide, N-(2-methoxy-5-nitrophenyl)-

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

504 g (3 mol) of 2-amino-4-nitro-1-methoxybenzene are introduced into 860 ml of acetic acid and 600 ml of water (or the combined main filtrate and first wash filtrate of a previous batch) and the mixture is heated to 80° C. 358 g (3.2 mol) of acetic anhydride are added dropwise in the course of 10 minutes. The mixture is subsequently stirred at 80° C. for 4 hours, and then cooled to room temperature, while stirring, by removing the heating bath and finally to 15° C. The pale yellow needles which have precipitated are filtered off with suction, washed with 300 ml of 60% strength acetic acid and 1500 ml of water in several portions and dried.

Aufarbeitung

  1. temperaturecooled to room temperature
  2. stirringwhile stirring
  3. customby removing the heating bath
  4. customfinally to 15° C
  5. customThe pale yellow needles which have precipitated
  6. filtrationare filtered off with suction
  7. washwashed with 300 ml of 60% strength acetic acid and 1500 ml of water in several portions
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-81e010c1cada4efabc4550a7a913a1fe
Quelldatensatz
uspto-grants-1995_02
Patentnummer
US05387716

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