反応 #61830

反応方程式

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

溶媒

2-methoxy-ethanol

反応条件

後処理

1. 1
   その他prepared
2. 2
   その他irradiation at 180° C.
3. 3
   その他The solvent was removed in vacuo
4. 4
   その他the residue was purified by silica gel chromatography
5. 5
   洗浄eluting with 50% EtOAc/hexane

実験手順

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).

出典