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Potassium Iodide → 6-chloro-1,3-dihydro-1-{3-[4-(1,3-dihydro-2-oxo-2H-benzimidazol-1-yl)-1-piperidinyl]propyl}-2H-benzimidazol-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 1,3-Dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-one | HCID 88638 | — |
| 反応物 | 6-chloro-1-(3-chloropropyl)-1,3-dihydro-2H-benzimidazol-2-one | HCID 20385587 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Methyl Isobutyl Ketone | HCID 7909 | — |
| 生成物 | 6-chloro-1,3-dihydro-1-{3-[4-(1,3-dihydro-2-oxo-2H-benzimidazol-1-yl)-1-piperidinyl]propyl}-2H-benzimidazol-2-one | HCID 20385612 | — |
反応手順
A mixture of 5.6 parts of 6-chloro-1-(3-chloropropyl)-1,3-dihydro-2H-benzimidazol-2-one, 4.34 parts of 1,3-dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-one, 6.4 parts of sodium carbonate, 0.2 parts of potassium iodide and 200 parts of 4-methyl-2-pentanone is stirred and refluxed overnight with water-separator. The reaction mixture is cooled and water is added. The undissolved product is filtered off and crystallized from a mixture of N,N-dimethylformamide and water. It is filtered off again, boiled in methanol, filtered off while hot and dried, yielding 5.1 parts of 6-chloro-1,3-dihydro-1-{3-[4-(1,3-dihydro-2-oxo-2H-benzimidazol-1-yl)-1-piperidinyl]propyl}-2H-benzimidazol-2-one; mp. 273° 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-dd3720cc04dd4784a643272c0c5d7ffa |
| 出典メモ | uspto-grants-1979_11 |