Hydrochloric Acid → HCID 58259952, Verbindung

HRID 598408Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 598408
[NH2:1][C:2]1[C:3]([NH:10][C:11]2[CH:16]=[CH:15][C:14]([I:17])=[CH:13][C:12]=2[F:18])=[CH:4][C:5](=[O:9])[N:6]([CH3:8])[CH:7]=1.[CH2:19]([C:22]1([S:25](Cl)(=[O:27])=[O:26])[CH2:24][CH2:23]1)[CH:20]=[CH2:21].Cl>N1C=CC=CC=1>[CH2:19]([C:22]1([S:25]([NH:1][C:2]2[C:3]([NH:10][C:11]3[CH:16]=[CH:15][C:14]([I:17])=[CH:13][C:12]=3[F:18])=[CH:4][C:5](=[O:9])[N:6]([CH3:8])[CH:7]=2)(=[O:27])=[O:26])[CH2:24][CH2:23]1)[CH:20]=[CH2:21]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 441819591-(Prop-2-en-1-yl)cyclopropane-1-sulfonyl chlorideHCID 58990848HCID 58990848, Verbindung

Produkt 1

HCID 58259952HCID 58259952, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

5-Amino-4-(2-fluoro-4-iodophenylamino)-1-methylpyridin-2(1H)-one (prepared as described in steps a-e in example 1 above) was dissolved in dry pyridine at 0° C. under an ice-salt bath, and 1-allylcyclopropane-1-sulfonyl chloride was added. The resultant reaction mixture was allowed to warm to room temperature. After stirring for 16 hours at room temperature, aqueous HCl (1N) was added and the mixture was stirred for 15 minutes. The formed precipitate was filtered and dried under vacuum, and purified by preparative TLC (SiO2, EtOAc:MeOH=9:1 (v:v), Rf ˜0.4).

Aufarbeitung

  1. customThe resultant reaction mixture
  2. stirringthe mixture was stirred for 15 minutes
  3. filtrationThe formed precipitate was filtered
  4. customdried under vacuum
  5. custompurified by preparative TLC (SiO2, EtOAc:MeOH=9:1 (v:v), Rf ˜0.4)

Quellen und Nachweise

ORD-Eintrag
ord-85aad6b6bf194be495e8d9908e1d5c0b
Quelldatensatz
uspto-grants-2011_03
Patentnummer
US07897624B2

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