Diethyl Ether → 4-Amino-6-(1-cyclopropylethyl)-3-methylthio-1,2,4-triazin-5(4H)-one

HRID 231388

Reaktionsgleichung

Reaktionsgleichung von HRID 231388
[NH2:1][N:2]1[C:7](=[O:8])[CH:6]([CH:9]([CH:11]2[CH2:13][CH2:12]2)[CH3:10])[NH:5][NH:4][C:3]1=[S:14].[OH-].[Na+].[CH3:17]COCC.CI>O>[NH2:1][N:2]1[C:7](=[O:8])[C:6]([CH:9]([CH:11]2[CH2:12][CH2:13]2)[CH3:10])=[N:5][N:4]=[C:3]1[S:14][CH3:17]

Komponenten

6

Edukt 4

HCID 3283Diethyl EtherHCID 6328Methyl iodideHCID 14798Sodium HydroxideHCID 200323464-amino-6-(1-cyclopropylethyl)-5-oxo-3-thioxo-tetrahydro-1,2,4-(2H,4H)-triazine

Produkt 1

HCID 144026044-Amino-6-(1-cyclopropylethyl)-3-methylthio-1,2,4-triazin-5(4H)-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
10 °C

Versuchsvorschrift

(according to process A): ##STR19## 789 g (3.72 mols) of 4-amino-6-(1-cyclopropylethyl)-5-oxo-3-thioxo-tetrahydro-1,2,4-(2H,4H)-triazine are dissolved in a solution of 151 g (3.77 mols) of sodium hydroxide in 4 l of water. 3 ml of alkylarylpolyglycol ether are added, the mixture is cooled to 10° C., 542 g (3.82 mols) of methyl iodide are added and the mixture is stirred for 4 hours at room temperature. The mixture is filtered off with suction and the residue is washed with water and also with petroleum ether and dried at 60° C. in vacuo, after which 748 g (89% of theory) of the above compound of melting point 111°-113° C. are obtained. The purity as determined by gas chromatography is 99%.

Aufarbeitung

  1. filtrationThe mixture is filtered off with suction
  2. washthe residue is washed with water and also with petroleum ether
  3. customdried at 60° C. in vacuo
  4. customafter which 748 g (89% of theory) of the above compound of melting point 111°-113° C. are obtained

Quellen und Nachweise

ORD-Eintrag
ord-d86555656bb547e39ba2cc995b5830ca
Quelldatensatz
uspto-grants-1989_07
Patentnummer
US04846881

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