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Methyl Isobutyl Ketone → 1-{1-[3-(1H-benzimidazol-1-yl)propyl]-4-piperidinyl}-5-chloro-1,3-dihydro-2H-benzimidazol-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl Isobutyl Ketone | HCID 7909 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 5-Chloro-1,3-dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-one | HCID 104607 | — |
| 反応物 | 1-(3-Chloropropyl)-1H-benzimidazole | HCID 13105517 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-{1-[3-(1H-benzimidazol-1-yl)propyl]-4-piperidinyl}-5-chloro-1,3-dihydro-2H-benzimidazol-2-one | HCID 20385579 | 14% |
反応手順
A mixture of 9 parts of 1-(3-chloropropyl)-1H-benzimidazole, 10 parts of 5-chloro-1,3-dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-one, 7.4 parts of sodium carbonate and 200 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 crystallized from 4-methyl-2-pentanone, yielding 2.9 parts (14%) of 1-{1-[3-(1H-benzimidazol-1-yl)propyl]-4-piperidinyl}-5-chloro-1,3-dihydro-2H-benzimidazol-2-one; mp. 224° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04175129 |
| 出典データセット | uspto-grants-1979_11 |
| ORD ID | ord-e14ae101c17d401ab38a545c8ba86135 |
| 出典メモ | uspto-grants-1979_11 |