Sodium Hydroxide → 7,8-Dihydro-5-(3,4-dimethoxyphenyl)-8-methyl-7-(2,4,6-trimethylphenylimino)-1,2,4-triazolo[4,3-a]pyrimidine

HRID 4332

Reaktionsgleichung

Reaktionsgleichung von HRID 4332
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[N:16]=[C:15]([NH:17][NH:18][CH:19]=O)[N:14]([CH3:21])[C:13](=[N:22][C:23]3[C:28]([CH3:29])=[CH:27][C:26]([CH3:30])=[CH:25][C:24]=3[CH3:31])[CH:12]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[OH-].[Na+]>O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[N:16]3[CH:19]=[N:18][N:17]=[C:15]3[N:14]([CH3:21])[C:13](=[N:22][C:23]3[C:28]([CH3:29])=[CH:27][C:26]([CH3:30])=[CH:25][C:24]=3[CH3:31])[CH:12]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 201523173,4-Dihydro-6-(3,4-dimethoxyphenyl)-2-(2-formylhydrazino)-3-methyl-4-(2,4,6-trimethylphenylimino)pyrimidine

Produkt 1

HCID 201523037,8-Dihydro-5-(3,4-dimethoxyphenyl)-8-methyl-7-(2,4,6-trimethylphenylimino)-1,2,4-triazolo[4,3-a]pyrimidineAusbeute 83,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

The mixture of 3,4-dihydro-6-(3,4-dimethoxyphenyl)-2-(2-formylhydrazino)-3-methyl-4-(2,4,6-trimethylphenylimino)pyrimidine (0.81 g) and polyphosphoric acid (8.2 g, 116% as phosphoric acid) was stirred at 110° C. for 2 hours and cooled to ambient temperature. The reaction mixture was poured into water and neutralized with aqueous sodium hydroxide solution. The precipitates were collected by filtration and washed with water to give 7,8-dihydro-5-(3,4-dimethoxyphenyl)-8-methyl-7-(2,4,6-trimethylphenylimino)-1,2,4-triazolo[4,3-a]pyrimidine (0.65 g).

Aufarbeitung

  1. temperaturecooled to ambient temperature
  2. filtrationThe precipitates were collected by filtration
  3. washwashed with water

Quellen und Nachweise

ORD-Eintrag
ord-9337e50ccd674af7a4a11996c30facfa
Quelldatensatz
uspto-grants-1988_02
Patentnummer
US04725600

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