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Pyridine → Pyrazosulfuron-ethyl

HRID 374571
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 374571
[O-:1][C:2]#[N:3].[Na+].[NH2:5][C:6]1[N:11]=[C:10]([O:12][CH3:13])[CH:9]=[C:8]([O:14][CH3:15])[N:7]=1.N1C=CC=CC=1.[CH3:22][N:23]1[C:27]([S:28](Cl)(=[O:30])=[O:29])=[C:26]([C:32]([O:34][CH2:35][CH3:36])=[O:33])[CH:25]=[N:24]1>C(#N)C>[CH3:13][O:12][C:10]1[CH:9]=[C:8]([O:14][CH3:15])[N:7]=[C:6]([NH:5][C:2]([NH:3][S:28]([C:27]2[N:23]([CH3:22])[N:24]=[CH:25][C:26]=2[C:32]([O:34][CH2:35][CH3:36])=[O:33])(=[O:30])=[O:29])=[O:1])[N:11]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 1049PyridineHCID 1189462-Amino-4,6-dimethoxypyrimidineHCID 517096Sodium CyanateHCID 10977963ethyl 5-(chlorosulfonyl)-1-methyl-1H-pyrazole-4-carboxylate

Produkt 1

HCID 91750Pyrazosulfuron-ethylAusbeute 98 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342
Acetonitrile
Lösungsmittel

Reaktionsbedingungen

Temperatur
45 °C

Versuchsvorschrift

7.27 g of anhydrous sodium cyanate, 15.78 g of 2-amino-4,6-dimethoxypyrimidine, 8.04 g of pyridine and 40 g of dry acetonitrile were mixed together and the mixture was warmed to 45° C. under nitrogen atmosphere. To this mixture was added 28.46 g of 1-methyl-4-ethoxycarbonylpyrazole-5-sulfonylchloride over 2 hours and the reaction mixture was stirred for further 2 hours while maintaining the temperature of 45° C. After the completion of the reaction was identified by liquid chromatography, the reaction product was extracted with 200 g of dichloromethane and 40 g of 5% aqueous sulfuric acid solution. The extracted organic layer was dried over anhydrous magnesium sulfate and then filtered. The organic solvent was removed from the product to obtain 41.30 g (Yield 98%) of the title compound as a solid state.

Aufarbeitung

  1. temperaturewhile maintaining the temperature of 45° C
  2. extractionthe reaction product was extracted with 200 g of dichloromethane and 40 g of 5% aqueous sulfuric acid solution
  3. dry with materialThe extracted organic layer was dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customThe organic solvent was removed from the product

Quellen und Nachweise

ORD-Eintrag
ord-b46e1e80933241f0a5c255e73e389dc5
Quelldatensatz
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05480993

Notizen zur Reaktion

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