참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Iodide | HCID 4875 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 5-Chloro-1,3-dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-one | HCID 104607 | — |
| 반응물 | 1-(3-chloropropyl)-1,3-dihydro-2H-benzimidazol-2-one | HCID 1810419 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Methyl Isobutyl Ketone | HCID 7909 | — |
| 생성물 | Domperidone | HCID 3151 | 30% |
반응 단계
A mixture of 2.3 parts of 1-(3-chloropropyl)-1,3-dihydro-2H-benzimidazol-2-one, 2.5 parts of 5-chloro-1,3-dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-one, 3.2 parts of sodium carbonate, 0.1 parts of potassium iodide and 80 parts of 4-methyl-2-pentanone is stirred and refluxed for 24 hours. The reaction mixture is cooled to room temperature and water is added. The undissolved product is filtered off and purified by column-chromatography over silica gel using a mixture of trichloromethane and 10% of methanol as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized from 4-methyl-2-pentanone. The product is filtered off and recrystallized from a mixture of N,N-dimethylformamide and water, yielding 1.3 parts (30%) of 5-chloro-1-{1-[3-(1,3-dihydro-2-oxo-2H-benzimidazol-1-yl)propyl]-4-piperidinyl}-1,3-dihydro-2H-benzimidazol-2-one; mp. 242.5° 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-c3e33f9cdb1a4315a7624b02e179c075 |
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| 출처 메모 | uspto-grants-1979_11 |
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