참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Iodide | HCID 4875 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 1-Phenyl-1,3,8-triazaspiro(4.5)decan-4-one | HCID 70556 | — |
| 반응물 | 1-(3-Chloropropyl)-1H-benzimidazole | HCID 13105517 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Methyl Isobutyl Ketone | HCID 7909 | — |
| 생성물 | 8-[3-(1H-benzimidazol-1-yl)propyl]-1-phenyl-1,3,8-triazaspiro[4,5]decan-4-one | HCID 20385639 | 25% |
반응 단계
A mixture of 6 parts of 1-(3-chloropropyl)-1H-benzimidazole, 4.6 parts of 1-phenyl-1,3,8-triazaspiro[4,5]decan-4-one, 10 parts of sodium carbonate, 0.1 parts of potassium iodide and 80 parts of 4-methyl-2-pentanone is stirred and refluxed overnight. The reaction mixture is cooled, water is added and the layers are separated. The organic phase is dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (90:10 by volume) as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized from 4-methyl-2-pentanone, yielding 2parts (25%) of 8-[3-(1H-benzimidazol-1-yl)propyl]-1-phenyl-1,3,8-triazaspiro-[4,5]decan-4-one; mp. 191° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04175129 |
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| 출처 데이터셋 | uspto-grants-1979_11 |
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| ORD ID | ord-d97cbc76753b4a4eba775885524be3cb |
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| 출처 메모 | uspto-grants-1979_11 |
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