Acetic Acid → HCID 178492408, Verbindung

HRID 613951

Reaktionsgleichung

Reaktionsgleichung von HRID 613951
C([N:4]1[C:8]2=[CH:9][C:10]([CH3:12])=[N:11][N:7]2[C:6]([C:13]2[CH:14]=[C:15]([NH:21][C:22](=[O:40])[C:23]3[CH:28]=[C:27]([N:29]=[N:30][C:31]4[CH:36]=[CH:35][C:34]([O:37][CH3:38])=[CH:33][CH:32]=4)[CH:26]=[CH:25][C:24]=3[OH:39])[CH:16]=[CH:17][C:18]=2[O:19][CH3:20])=[N:5]1)(=O)C.[OH-].[Na+].C(O)(=O)C>CO.O>[CH3:20][O:19][C:18]1[CH:17]=[CH:16][C:15]([NH:21][C:22](=[O:40])[C:23]2[CH:28]=[C:27]([N:29]=[N:30][C:31]3[CH:32]=[CH:33][C:34]([O:37][CH3:38])=[CH:35][CH:36]=3)[CH:26]=[CH:25][C:24]=2[OH:39])=[CH:14][C:13]=1[C:6]1[N:7]2[N:11]=[C:10]([CH3:12])[CH:9]=[C:8]2[NH:4][N:5]=1

Komponenten

6

Edukt 3

HCID 176Acetic AcidHCID 14798Sodium HydroxideHCID 136398787N-[3-(1-Acetyl-6-methyl-1H-pyrazolo[3,2-c]-s-triazol-3-yl)-4-methoxyphenyl]-2-hydroxy-5-(4-methoxyphenylazo) benzamide

Produkt 1

HCID 178492408HCID 178492408, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

N-[3-(1-Acetyl-6-methyl-1H-pyrazolo[3,2-c]-s-triazol-3-yl)-4-methoxyphenyl]-2-hydroxy-5-(4-methoxyphenylazo)benzamide (1.4 g) was dissolved in methanol (100 ml) and a solution of sodium hydroxide (1.0 g) in water (30 ml) added. After stirring for 15 minutes the solution was acidified with glacial acetic acid when a gelatinous precipitate of the product appeared. This was removed by filtration, washed with water and crystallized in aqueous pyridine (850 mg; 66%), m.p. 295°-6°, λmax (methanol) = 350 nm.

Aufarbeitung

  1. customThis was removed by filtration
  2. washwashed with water
  3. customcrystallized in aqueous pyridine (850 mg; 66%)

Quellen und Nachweise

ORD-Eintrag
ord-d404be490dec415fac71eb764a609577
Quelldatensatz
uspto-grants-1979_03
Patentnummer
US04142901

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