5,6,7,8-Tetrahydronaphthalene-1,7-diol → HCID 178515618, Verbindung

HRID 33552

Reaktionsgleichung

Reaktionsgleichung von HRID 33552
Cl[C:2]1[NH:6][C:5]2[CH:7]=[CH:8][C:9]([C:11]([F:14])([F:13])[F:12])=[CH:10][C:4]=2[N:3]=1.[C:15]1([OH:26])[C:24]2[CH2:23][CH:22]([OH:25])[CH2:21][CH2:20][C:19]=2[CH:18]=[CH:17][CH:16]=1>COCCO>[F:12][C:11]([F:14])([F:13])[C:9]1[CH:8]=[CH:7][C:5]2[NH:6][C:2]([O:26][C:15]3[CH:16]=[CH:17][CH:18]=[C:19]4[C:24]=3[CH2:23][CH:22]([OH:25])[CH2:21][CH2:20]4)=[N:3][C:4]=2[CH:10]=1

Komponenten

4

Edukt 2

HCID 124457395,6,7,8-Tetrahydronaphthalene-1,7-diolHCID 178506089HCID 178506089, Verbindung

Produkt 1

HCID 178515618HCID 178515618, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 80192-MethoxyethanolLösungsmittel

Versuchsvorschrift

A mixture of 2-chloro-5-(trifluoromethyl)-1H-benzo[d]imidazole (89 mg, 0.4 mol, prepared according to the procedure described in WO 2004/035549 A1), 5,6,7,8-tetrahydronaphthalene-1,7-diol from step (a) above (49 mg, 0.3 mmol) and 2-methoxy-ethanol (1 mL, Aldrich) was subjected to microwave irradiation at 180° C. with stirring for 60 min twice. The solvent was removed in vacuo and the residue was purified by silica gel chromatography, eluting with 50% EtOAc/hexane to give the title compound as an amorphous solid. MS (ESI, pos. ion) m/z: 349 (M+1).

Aufarbeitung

  1. customprepared
  2. customirradiation at 180° C.
  3. customThe solvent was removed in vacuo
  4. customthe residue was purified by silica gel chromatography
  5. washeluting with 50% EtOAc/hexane

Quellen und Nachweise

ORD-Eintrag
ord-e7f5a3b6bf3c409fb2ace8e43952cc6f
Quelldatensatz
uspto-grants-2008_09
Patentnummer
US07429608B2

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