반응 #78394
ord-99fa2889009c44f08cb79bded6f748b6
반응 방정식
반응물
시약
없음
용매
반응 조건
온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도was refluxed for 9 h
- 2여과filtered
- 3농축The filtrate was concentrated to a volume of 30 ml under diminished pressure
- 4workup.ADDITIONafter addition of 150 ml of acetonitrile again to a volume
- 5여과the precipitated crystals were filtered
- 6세척washed twice with 25 ml of cold acetonitrile
- 7기타dried at 70° C.
실험 절차
In a 500 ml flask a mixture of 200 ml of dry ethanol, 20 g (0.026 mol) of 2-n-butyl-4-chloro-1-[(2′-(2-triphenylmethyl -2H-tetrazol-5-yl)-1,1′-biphenyl-4-yl)-methyl]1H-imidazol-5-methanol methyl-isobutyl ketone solvate and 1.45 g (0.026 mol) of potassium hydroxide was refluxed for 9 h, treated with 0.5 g of charcoal and filtered. The filtrate was concentrated to a volume of 30 ml under diminished pressure, and after addition of 150 ml of acetonitrile again to a volume: of 60 ml. The suspension was stirred at 0° C. for 1 h, the precipitated crystals were filtered, washed twice with 25 ml of cold acetonitrile and dried at 70° C. to give 10.6 g (88%) of the title compound.