Sodium Hydroxide → HCID 23469722, Verbindung

HRID 128464

Reaktionsgleichung

Reaktionsgleichung von HRID 128464
Cl.[F:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH:9][NH2:10].[OH-].[Na+].CN([CH:16]=[N:17][C:18](=O)[C:19]1[CH:24]=[CH:23][C:22]([N+:25]([O-:27])=[O:26])=[CH:21][CH:20]=1)C>O.O1CCOCC1.C(O)(=O)C>[F:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[C:18]([C:19]2[CH:20]=[CH:21][C:22]([N+:25]([O-:27])=[O:26])=[CH:23][CH:24]=2)=[N:17][CH:16]=[N:10]1

Komponenten

7

Edukt 3

HCID 14798Sodium HydroxideHCID 2723910Hydrazine, (2-fluorophenyl)-, hydrochloride (1:1)HCID 12550338HCID 12550338, Verbindung

Produkt 1

HCID 23469722HCID 23469722, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittel2×HCID 312751,4-DioxaneLösungsmittel2×

Versuchsvorschrift

A 25.0 g. portion of o-fluorophenylhydrazine hydrochloride is dissolved in 150 ml. of p-dioxane with warming and 31.0 ml. of 5 N sodium hydroxide is added. After solution is complete, 80 ml. of glacial acetic acid and 210 ml. of water are added followed by 28.1 g. of N-(dimethylaminomethylene)-p-nitrobenzamide in 100 ml. of warm p-dioxane. This reaction mixture is heated at 90°-95° C. for 1.5 hours, then cooled and poured into 1500 ml. of water. The solid is collected by filtration, washed with water, dried and crystallized from 200 ml. of ethanol, giving 13.9 g. of the desired product as a tan solid, mp. 143°-145° C.

Aufarbeitung

  1. temperatureThis reaction mixture is heated at 90°-95° C. for 1.5 hours
  2. temperaturecooled
  3. additionpoured into 1500 ml
  4. filtrationThe solid is collected by filtration
  5. washwashed with water
  6. customdried
  7. customcrystallized from 200 ml
  8. customof ethanol, giving 13.9 g

Quellen und Nachweise

ORD-Eintrag
ord-769e086f96e04461b8f8105605192835
Quelldatensatz
uspto-grants-1981_03
Patentnummer
US04259504

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