反应详情

Under nitrogen, in a 500 ml flask a mixture of 180 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 0.1 g (0.00178 mol) of potassium hydroxide was refluxed for 3 h. The reaction mixture was cooled to room temperature and after adding 1.35 g (0.0241 mol) of potassium hydroxide in 10 ml of methanol it was 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 80 ml of acetonitrile again to a volume of 35 ml. After addition of further 85 ml of acetonitrile the suspension was cooled to 0° C., the precipitated crystals were filtered after 1 h stirring, washed twice with 30 ml of cold acetonitrile and dried at 70° C. to give 11.3 g (93.4%) of the title compound.

1. temperaturewas refluxed for 3 h
2. filtrationfiltered
3. concentrationThe filtrate was concentrated to a volume of 30 ml under diminished pressure
4. additionafter addition of 80 ml of acetonitrile again to a volume of 35 ml
5. additionAfter addition of further 85 ml of acetonitrile the suspension
6. temperaturewas cooled to 0° C.
7. filtrationthe precipitated crystals were filtered after 1 h
8. washwashed twice with 30 ml of cold acetonitrile
9. customdried at 70° C.