Hydrochloric Acid → 6-[(4-Chlorobenzene-1-sulfonyl)(2,5-difluorophenyl)methyl]pyridin-2-amine

HRID 2080444Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2080444
C(O)C.C(OC(=O)[NH:10][C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([CH:17]([S:26]([C:29]2[CH:34]=[CH:33][C:32]([Cl:35])=[CH:31][CH:30]=2)(=[O:28])=[O:27])[C:18]2[CH:23]=[C:22]([F:24])[CH:21]=[CH:20][C:19]=2[F:25])[N:12]=1)(C)(C)C.Cl>C(OCC)(=O)C>[Cl:35][C:32]1[CH:33]=[CH:34][C:29]([S:26]([CH:17]([C:18]2[CH:23]=[C:22]([F:24])[CH:21]=[CH:20][C:19]=2[F:25])[C:13]2[N:12]=[C:11]([NH2:10])[CH:16]=[CH:15][CH:14]=2)(=[O:28])=[O:27])=[CH:30][CH:31]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 58734259HCID 58734259, Verbindung

Produkt 1

HCID 231147766-[(4-Chlorobenzene-1-sulfonyl)(2,5-difluorophenyl)methyl]pyridin-2-amineAusbeute 71,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To an ethanol (5 ml) solution of t-butyl[6-[(4-chlorophenylsulfonyl)(2,5-difluorophenyl)methyl]pyridin-2-yl]carbamate (370 mg, 0.748 mmol) was added concentrated hydrochloric acid (5 ml). The resulting mixture was stirred at room temperature for 6 hours. The reaction mixture was concentrated under reduced pressure. To the residue thus obtained was added ethyl acetate. The resulting mixture was washed sequentially with saturated sodium bicarbonate and brine. The organic layer thus obtained was dried over magnesium sulfate and concentrated under reduced pressure to give the title compound (210 mg, 0.537 mmol, 71%) as a white powder.

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customTo the residue thus obtained
  3. washThe resulting mixture was washed sequentially with saturated sodium bicarbonate and brine
  4. customThe organic layer thus obtained
  5. dry with materialwas dried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-e1bebf0f496f423280319a2e0b3271ea
Quelldatensatz
uspto-grants-2011_04
Patentnummer
US07932271B2

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