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Sulfuric Acid → HCID 72312730, Verbindung

HRID 1161371
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1161371
N1C(C)=CC(C)=CC=1C.Cl[C:11]([O:13][CH3:14])=[O:12].[CH3:15][S:16][C:17](=[NH:39])[C:18](=[N:30][C:31]1[CH:36]=[CH:35][C:34]([C:37]#[N:38])=[CH:33][CH:32]=1)[C:19]1[CH:24]=[C:23]([O:25][CH3:26])[CH:22]=[C:21]([O:27][CH3:28])[C:20]=1[F:29].S(=O)(=O)(O)O>C1(C)C=CC=CC=1.C(OCC)(=O)C>[CH3:14][O:13][C:11](=[O:12])[N:39]=[C:17]([S:16][CH3:15])[C:18](=[N:30][C:31]1[CH:36]=[CH:35][C:34]([C:37]#[N:38])=[CH:33][CH:32]=1)[C:19]1[CH:24]=[C:23]([O:25][CH3:26])[CH:22]=[C:21]([O:27][CH3:28])[C:20]=1[F:29]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 1118Sulfuric AcidHCID 6586Methyl chloroformateHCID 79532,4,6-TrimethylpyridineHCID 59517045HCID 59517045, Verbindung

Produkt 1

HCID 72312730HCID 72312730, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1140Toluene
Lösungsmittel
HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
85 °C

Versuchsvorschrift

After adding 2.97 ml of 2,4,6-collidine and 1.74 ml of methyl chloroformate to a solution of 2.01 g of 2-(4-cyanophenylimino)-2-(2-fluoro-3,5-dimethoxyphenyl)thioacetimidic acid methyl ester in 80 ml of toluene, the mixture was stirred at 85° C. for 20 hours under a nitrogen atmosphere. After cooling the reaction mixture, 400 ml of ethyl acetate and 200 ml of a 2% aqueous sulfuric acid solution were added and the organic layer was washed with 300 ml of water and 300 ml of saturated brine. The organic layer was dried over anhydrous magnesium sulfate, the desiccating agent was filtered off and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (heptane-ethyl acetate (3:2)) to give the title compound (1.89 g) as a light yellow solid.

Aufarbeitung

  1. additionwere added
  2. washthe organic layer was washed with 300 ml of water and 300 ml of saturated brine
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. filtrationthe desiccating agent was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (heptane-ethyl acetate (3:2))

Quellen und Nachweise

ORD-Eintrag
ord-6bae17e8ab674faf90db9130a2221801
Quelldatensatz
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07816522B2

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