反应详情

Under nitrogen, in a 500 ml flask a mixture of 175 ml of dry methanol, 20 g (0.026 mol) of 2-n-butyl-4-chloro 1-[(2′-(2-triphenylmethyl-2H-tetrazol-5-yl)-1,1′biphenyl-4-yl)-me thyl]-1H-imidazol-5-methanol methyl-isobutyl ketone solvate and 1.46 g (0.026 mol) of potassium hydroxide in 25 ml of methanol was warmed to reflux temperature over a period of 30 min. After refluxing for 4 h, the reaction was cooled to room temperature, treated with 0.6 g of charcoal and filtered. The filtrate was concentrated to a volume of 30-35 ml under diminished pressure, and after addition of 85 ml of acetonitrile again to a volume of 30-35 ml. After addition of further 85 ml of acetonitrile the solution is concentrated to a volume of 60-65 ml. The suspension was stirred at 0−(+)2° C. for 2 h, the precipitated crystals were filtered, washed three times with 30 ml of cold acetonitrile and dried at 70° C. to give 11.5 g (94%) of the title compound.

1. temperaturewas warmed
2. temperatureto reflux temperature over a period of 30 min
3. temperatureAfter refluxing for 4 h
4. filtrationfiltered
5. concentrationThe filtrate was concentrated to a volume of 30-35 ml under diminished pressure
6. additionafter addition of 85 ml of acetonitrile again to a volume of 30-35 ml
7. additionAfter addition of further 85 ml of acetonitrile the solution
8. concentrationis concentrated to a volume of 60-65 ml
9. filtrationthe precipitated crystals were filtered
10. washwashed three times with 30 ml of cold acetonitrile
11. customdried at 70° C.