Reaktion #61830

Reaktionsgleichung

2-chloro-5-(trifluoromethyl)-1H-benzo[d]imidazole

5,6,7,8-tetrahydronaphthalene-1,7-diol

→

title compound

8-(5-(Trifluoromethyl)-1H-benzo[d]imidazol-2-yloxy)-1,2,3,4-tetrahydronaphthalen-2-ol

Lösungsmittel

2-methoxy-ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeprepared
2. 2
   Sonstigeirradiation at 180° C.
3. 3
   SonstigeThe solvent was removed in vacuo
4. 4
   Sonstigethe residue was purified by silica gel chromatography
5. 5
   Wascheneluting with 50% EtOAc/hexane

Vorschrift

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).

Quelle