Water → Ethyl[3-(6-oxo-3-thiocarbamoyl-6h-pyridazin-1-yl-methyl)phenyl]carbamate

HRID 383644

Reaktionsgleichung

Reaktionsgleichung von HRID 383644
[CH2:1]([O:3][C:4](=[O:22])[NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([CH2:12][N:13]2[C:18](=[O:19])[CH:17]=[CH:16][C:15]([C:20]#[N:21])=[N:14]2)[CH:7]=1)[CH3:2].[Cl-].C([NH2+]CC)C.O.[S-2:30].[Na+].[Na+].O>CN(C=O)C>[CH2:1]([O:3][C:4](=[O:22])[NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([CH2:12][N:13]2[C:18](=[O:19])[CH:17]=[CH:16][C:15]([C:20](=[S:30])[NH2:21])=[N:14]2)[CH:7]=1)[CH3:2]

Komponenten

6

Edukt 4

HCID 962WaterHCID 12618Diethylamine, hydrochlorideHCID 19906495Sodium sulfide monohydrateHCID 59406667Ethyl[3-(3-cyano-6-oxo-6H-pyridazin-1-ylmethyl)phenyl]-carbamate

Produkt 1

HCID 59406698Ethyl[3-(6-oxo-3-thiocarbamoyl-6h-pyridazin-1-yl-methyl)phenyl]carbamate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
55 °C

Versuchsvorschrift

200 mg (0.67 mmol) of ethyl[3-(3-cyano-6-oxo-6H-pyridazin-1-ylmethyl)-phenyl]carbamate are dissolved in 1 ml of DMF, and 219 mg (2 mmol) of diethylammonium chloride and 165 mg (2 mmol) of sodium sulfide hydrate are added. The yellow suspension is stirred at 55° C. for 2 hours. 10 ml of water are added to the reaction mixture. The precipitate is filtered off with suction, washed with water and dried in vacuo. The substance is reacted further without further purification.

Aufarbeitung

  1. filtrationThe precipitate is filtered off with suction
  2. washwashed with water
  3. customdried in vacuo
  4. customThe substance is reacted further without further purification

Quellen und Nachweise

ORD-Eintrag
ord-31010b8f76d946b3b04a246806827eee
Quelldatensatz
uspto-grants-2013_02
Patentnummer
US08367668B2

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