참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methane | HCID 297 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | 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 | HCID 69886909 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | Losartan potassium salt | HCID 11476710 | 95.9% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06710183B2 |
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| 출처 데이터셋 | uspto-grants-2004_03 |
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| ORD ID | ord-6022181667ea4138a8f6aead0a43b0a4 |
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| 출처 메모 | uspto-grants-2004_03 |
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