Hydroxylamine → HCID 21919395, Verbindung

HRID 1581941Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1581941
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[CH2:13][CH2:12][N:11]([S:14](/[CH:17]=[CH:18]/[CH2:19][CH2:20][C:21]3[N:26]=[CH:25][C:24]([F:27])=[CH:23][N:22]=3)(=[O:16])=[O:15])[CH2:10][CH2:9]2)=[N:6][CH:7]=1.ClC1C=CC(N2CCN(S(/C=C\CCC3N=CC(F)=CN=3)(=O)=O)CC2)=NC=1.[NH2:55][OH:56]>O1CCCC1.CCOC(C)=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[CH2:13][CH2:12][N:11]([S:14]([CH2:17][CH:18]([NH:55][OH:56])[CH2:19][CH2:20][C:21]3[N:26]=[CH:25][C:24]([F:27])=[CH:23][N:22]=3)(=[O:16])=[O:15])[CH2:10][CH2:9]2)=[N:6][CH:7]=1

Komponenten

6

Edukt 3

HCID 787HydroxylamineHCID 21919407HCID 21919407, VerbindungHCID 69596186HCID 69596186, Verbindung

Produkt 1

HCID 21919395HCID 21919395, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8028TetrahydrofuranLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a solution of 2-((E)-4-[4-(5-chloropyridin-2-yl)piperazino]sulfonylbut-3-enyl)-5-fluoropyrimidine and 2-((Z)-4-[4-(5-chloropyridin-2-yl)piperazino]sulfonylbut-3-enyl)-5-fluoropyrimidine (0.44 g), in tetrahydrofuran (5 ml), was added hydroxylamine (1.0 ml, 50% aqueous solution). The mixture was stirred for 18 hours and then diluted with EtOAc (10 ml) and washed with saturated ammonium chloride solution (10 ml). The organic layer was dried over Na2SO4 and evaporated in vacuo to give 2-[4-[4-(5-chloropyridin-2-yl)piperazino]sulfonyl-3-(hydroxyamino)butyl]-5-fluoropyrimidine (0.483 g).

Aufarbeitung

  1. washwashed with saturated ammonium chloride solution (10 ml)
  2. dry with materialThe organic layer was dried over Na2SO4
  3. customevaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-8661a4b06e844750b1220944b21e3145
Quelldatensatz
uspto-grants-2004_05
Patentnummer
US06734183B2

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