반응 #78393

반응 방정식

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

potassium hydroxide

charcoal

→

title compound

수율 101.7%

Losartan Potassium

수율 101.7%

용매

methanol

methanol

반응 조건

후처리

1. 1
   온도was refluxed for 3 h
2. 2
   여과filtered
3. 3
   농축The filtrate was concentrated to a volume of 30 ml under diminished pressure
4. 4
   workup.ADDITIONafter addition of 80 ml of acetonitrile again to a volume of 35 ml
5. 5
   workup.ADDITIONAfter addition of further 85 ml of acetonitrile the suspension
6. 6
   온도was cooled to 0° C.
7. 7
   여과the precipitated crystals were filtered after 1 h
8. 8
   세척washed twice with 30 ml of cold acetonitrile
9. 9
   기타dried at 70° C.

실험 절차

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.

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