반응 #61830

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

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

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title compound

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

용매

2-methoxy-ethanol

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후처리

1. 1
   기타prepared
2. 2
   기타irradiation at 180° C.
3. 3
   기타The solvent was removed in vacuo
4. 4
   기타the residue was purified by silica gel chromatography
5. 5
   세척eluting with 50% EtOAc/hexane

실험 절차

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).

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