Water → 4-(methylthio)-1H-indazol-5-ol

HRID 1269926

Reaktionsgleichung

Reaktionsgleichung von HRID 1269926
FC(F)(F)C(O)=O.[CH3:8][S:9][C:10]1[C:18]([O:19]C2CCCCO2)=[CH:17][CH:16]=[C:15]2[C:11]=1[CH:12]=[N:13][N:14]2C1CCCCO1.O>ClCCl>[CH3:8][S:9][C:10]1[C:18]([OH:19])=[CH:17][CH:16]=[C:15]2[C:11]=1[CH:12]=[N:13][NH:14]2

Komponenten

5

Edukt 3

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 694312114-(methylthio)-1-tetrahydro-2H-pyran-2-yl-5-(tetrahydro-2H-pyran-2-yloxy)-1H-indazole

Produkt 1

HCID 229336484-(methylthio)-1H-indazol-5-olAusbeute 127,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Trifluoroacetic acid (1 ml) was added to a solution of 4-(methylthio)-1-tetrahydro-2H-pyran-2-yl-5-(tetrahydro-2H-pyran-2-yloxy)-1H-indazole (0.0730 g, 0.21 mmol) in dichloromethane (1 ml) and stirred for 1 hour. The reaction solution was added to water and extracted three times with ethyl acetate and the extract solution was dried over anhydrous magnesium sulfate. The solvent was distilled off and the residue was purified by a silica gel chromatography (hexane/ethyl acetate=2/1), crystallized from hexane/ethyl acetate and then dried up to obtain 4-(methylthio)-1H-indazol-5-ol (0.0481 g, >99%).

Aufarbeitung

  1. extractionextracted three times with ethyl acetate
  2. dry with materialthe extract solution was dried over anhydrous magnesium sulfate
  3. distillationThe solvent was distilled off
  4. customthe residue was purified by a silica gel chromatography (hexane/ethyl acetate=2/1)
  5. customcrystallized from hexane/ethyl acetate
  6. customdried up

Quellen und Nachweise

ORD-Eintrag
ord-859c810b4a29438a86d48865296117bc
Quelldatensatz
uspto-grants-2007_04
Patentnummer
US07199147B2

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