Sodium Hydroxide → 5-Amino-1-methyl-4-phenoxycarbonylaminopyrazole

HRID 1247803Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1247803
S(=O)(=O)(O)O.[NH2:6][C:7]1[CH:8]=[N:9][N:10]([CH3:13])[C:11]=1[NH2:12].[OH-].[Na+].O1CCOCC1.Cl[C:23]([O:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=[O:24]>O>[NH2:12][C:11]1[N:10]([CH3:13])[N:9]=[CH:8][C:7]=1[NH:6][C:23]([O:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=[O:24]

Komponenten

6

Edukt 4

HCID 14798Sodium Hydroxide2×HCID 15891Phenyl chloroformateHCID 312751,4-DioxaneHCID 219045711H-Pyrazole, 4,5-diamine-1-methyl-, sulfate (1:1)

Produkt 1

HCID 219044605-Amino-1-methyl-4-phenoxycarbonylaminopyrazoleAusbeute 88,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of 4,5-diamino-1-methylpyrazole sulfuric acid salt (158 g) in water (1.1 L) was neutralized to pH 6.9 with 4N aqueous sodium hydroxide solution, and dioxane (474 ml) was added to this solution. To the resulting mixture was added dropwise phenyl chloroformate (124 g) maintaining pH of the mixture at 6.9 with 4N aqueous sodium hydroxide solution at a temperature below 10° C. The reaction mixture was stirred for 1 hour. The precipitated solid was collected by filtration and dried to give 5-amino-1-methyl-4-phenoxycarbonylaminopyrazole (155 g).

Aufarbeitung

  1. additionwas added to this solution
  2. filtrationThe precipitated solid was collected by filtration
  3. customdried

Quellen und Nachweise

ORD-Eintrag
ord-3b2fadddf35c422fa9ceb26dbff1ecd5
Quelldatensatz
uspto-grants-2006_10
Patentnummer
US07129232B2

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