Hydrochloric Acid → HCID 13924322, Verbindung

HRID 2308613Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2308613
[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH2:11])(=[O:10])=[O:9])=[CH:4][CH:3]=1.[Cl:12][C:13]1[CH:14]=[C:15]([CH:19]=[C:20]([O:22][CH3:23])[N:21]=1)[C:16](Cl)=[O:17].Cl.CCCCCC.C(OC(=O)C)C>N1C=CC=CC=1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([S:8]([NH:11][C:16](=[O:17])[C:15]2[CH:19]=[C:20]([O:22][CH3:23])[N:21]=[C:13]([Cl:12])[CH:14]=2)(=[O:9])=[O:10])=[CH:6][CH:7]=1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 1202314-FluorobenzenesulfonamideHCID 27821252-chloro-6-methoxypyridine-4-carbonyl chlorideHCID 21226206Ethyl acetate hexane

Produkt 1

HCID 13924322HCID 13924322, VerbindungAusbeute 61 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

1.75 g (0.01 mol) of 4-fluorobenzenesulfonamide were dissolved in 30 ml of pyridine, and added dropwise by 2.06 g (0.01 mol) of 2-chloro-6-methoxyisonicotinoyl chloride at 0° C. to 5° C., followed by agitation for 2 hrs. at room temperature. After acidified by adding aqueous hydrochloric acid, the precipitate was extracted by ethyl acetate. The organic layer obtained was dried and them concentrated to precipitate crude crystals, which were recrystallized by n-hexane/ethylacetate to 2.1 g (yield: 61.0%) of N-(4-fluorophenylsulfonyl)-2-chloro-6-methoxy isonicotinamide as white crystal.

Aufarbeitung

  1. customat room temperature
  2. extractionthe precipitate was extracted by ethyl acetate
  3. customThe organic layer obtained
  4. customwas dried
  5. concentrationthem concentrated
  6. customto precipitate crude crystals, which

Quellen und Nachweise

ORD-Eintrag
ord-6be548f541cd42159275001e918b291d
Quelldatensatz
uspto-grants-1987_09
Patentnummer
US04690934

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