反应详情

温度

0 °C

Under nitrogen, in a 500 ml flask a mixture of 200 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) -methyl]-1H-imidazol-5-methanol methyl-isobutyl ketone solvate and 1.45 g (0.026 mol) of potassium hydroxide was refluxed for 3 h, treated with 0.4 g of charcoal and filtered at room temperature. The filtrate was concentrated to a volume of 30 ml under diminished pressure, and after addition of 160 ml of heptane again to a volume of 130 ml. The suspension was stirred at 0° C. for 2 h, the precipitated crystals were filtered, washed with cold heptane and dried at 70° C. to give 11.3 g (92.5%) of the title compound.

1. temperaturewas refluxed for 3 h
2. filtrationfiltered at room temperature
3. concentrationThe filtrate was concentrated to a volume of 30 ml under diminished pressure
4. additionafter addition of 160 ml of heptane again to a volume of 130 ml
5. filtrationthe precipitated crystals were filtered
6. washwashed with cold heptane
7. customdried at 70° C.