p-Toluenesulfonic acid monohydrate → HCID 22715041, Verbindung

HRID 352083

Reaktionsgleichung

Reaktionsgleichung von HRID 352083
[F:1][C:2]([F:34])([F:33])[C:3]1[CH:8]=[CH:7][C:6](/[CH:9]=[CH:10]/[C:11]2[O:12][CH:13]=[C:14]([CH2:16][O:17][C:18]3[CH:23]=[CH:22][C:21]([CH2:24][CH2:25][CH2:26][CH2:27][N:28]4[CH:32]=[CH:31][N:30]=[N:29]4)=[CH:20][CH:19]=3)[N:15]=2)=[CH:5][CH:4]=1.O.[C:36]1([CH3:46])[CH:41]=[CH:40][C:39]([S:42]([OH:45])(=[O:44])=[O:43])=[CH:38][CH:37]=1>C(OCC)(=O)C.O1CCCC1>[C:36]1([CH3:46])[CH:37]=[CH:38][C:39]([S:42]([OH:45])(=[O:43])=[O:44])=[CH:40][CH:41]=1.[F:34][C:2]([F:1])([F:33])[C:3]1[CH:4]=[CH:5][C:6](/[CH:9]=[CH:10]/[C:11]2[O:12][CH:13]=[C:14]([CH2:16][O:17][C:18]3[CH:23]=[CH:22][C:21]([CH2:24][CH2:25][CH2:26][CH2:27][N:28]4[CH:32]=[CH:31][N:30]=[N:29]4)=[CH:20][CH:19]=3)[N:15]=2)=[CH:7][CH:8]=1

Komponenten

5

Edukt 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 6444692Mubritinib

Produkt 1

HCID 22715041HCID 22715041, VerbindungAusbeute 80,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8028TetrahydrofuranLösungsmittel2×HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

1-[4-[4-[[2-[(E)-2-[4-(Trifluoromethyl)phenyl]ethenyl]-1,3-oxazol-4-yl]methoxy]phenyl]butyl]-1H-1,2,3-triazole (1.0 g) was dissolved in ethyl acetate (50 ml) and tetrahydrofuran (5 ml). A solution of p-toluenesulfonic acid monohydrate (406 mg) in tetrahydrofuran (5 ml) was added dropwise. The crystals were precipitated. The mixture was stirred at room temperature for 2 hours 20 min and filtrated. The mixture was washed with ethyl acetate/isopropyl ether=1/1 (3 ml) and dried under reduced pressure (40° C.) to give 1-[4-[4-[[2-[(E)-2-[4-(trifluoromethyl)phenyl]ethenyl]-1,3-oxazol-4-yl]methoxy]phenyl]butyl]-1H-1,2,3-triazole p-toluenesulfonate (1.1 g, yield 80%).

Aufarbeitung

  1. customThe crystals were precipitated
  2. filtrationfiltrated
  3. washThe mixture was washed with ethyl acetate/isopropyl ether=1/1 (3 ml)
  4. customdried under reduced pressure (40° C.)

Quellen und Nachweise

ORD-Eintrag
ord-83ea170c387d4a01b2e04dca1a9bf9a6
Quelldatensatz
uspto-grants-2004_06
Patentnummer
US06743924B2

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