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Sulfuric Acid → Pyrazosulfuron-ethyl

HRID 374572
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 374572
[CH2:1]([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([CH3:15])[C:10]=1[S:11](Cl)(=[O:13])=[O:12])=[O:5])[CH3:2].[O-:16][C:17]#[N:18].[Na+].[CH3:20][O:21][C:22]1[CH:27]=[C:26]([O:28][CH3:29])[N:25]=[C:24]([NH2:30])[N:23]=1.S(=O)(=O)(O)O>C(#N)C.ClCCl.N1C=CC=CC=1>[CH3:20][O:21][C:22]1[CH:27]=[C:26]([O:28][CH3:29])[N:25]=[C:24]([NH:30][C:17]([NH:18][S:11]([C:10]2[N:9]([CH3:15])[N:8]=[CH:7][C:6]=2[C:4]([O:3][CH2:1][CH3:2])=[O:5])(=[O:13])=[O:12])=[O:16])[N:23]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 1118Sulfuric AcidHCID 1189462-Amino-4,6-dimethoxypyrimidineHCID 517096Sodium CyanateHCID 10977963ethyl 5-(chlorosulfonyl)-1-methyl-1H-pyrazole-4-carboxylate

Produkt 1

HCID 91750Pyrazosulfuron-ethylAusbeute 99 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 1049
Pyridine
Lösungsmittel
HCID 6342AcetonitrileLösungsmittel
HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

2.603 g of 4-ethoxycarbonyl-1-methylpyrazole-5-sulfonylchloride was dissolved in 20.0 ml of acetonitrile. To the resulting solution were added 0.715 g of sodium cyanate and 1,552 g (10.0 mM) of 4,6-dimethoxy-2-aminopyrimidine with stirring. The reaction mixture was maintained at 40° C. for about 10 minutes and then 0.396 g of pyridine was added dropwise thereto over 5 minutes via a syringe. While maintaining the temperature of 40° to 45° C., the reaction mixture was continuously and vigorously stirred for 3 hours to complete the reaction. After the reaction was completed, the reaction mixture was adjusted to pH 4 by adding 5% aqueous sulfuric acid solution and dichloromethane to extract the reaction product. The extracted organic layer was dried over anhydrous magnesium sulfate and then filtered. The organic solvent was removed from the filtrate to obtain 4.103 g (Yield 99%) of the title compound in the solid state.

Aufarbeitung

  1. temperatureWhile maintaining the temperature of 40° to 45° C.
  2. stirringvigorously stirred for 3 hours
  3. customthe reaction
  4. extractionto extract the reaction product
  5. dry with materialThe extracted organic layer was dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. customThe organic solvent was removed from the filtrate

Quellen und Nachweise

ORD-Eintrag
ord-2bc992b923ee42249c60809a5e898a70
Quelldatensatz
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05480993

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