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1,3-Dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-one → ethyl 2-[4-(2,3-dihydro-2-oxo-1H-benzimidazol-1-yl)-1-piperidinyl]ethylcarbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,3-Dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-one | HCID 88638 | — |
| 反応物 | ethyl N-(2-bromoethyl)carbamate | HCID 286694 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | ethyl 2-[4-(2,3-dihydro-2-oxo-1H-benzimidazol-1-yl)-1-piperidinyl]ethylcarbamate | HCID 21428897 | — |
反応手順
A mixture of 12.94 parts of ethyl (2-bromoethyl)carbamate, 13.51 parts of 1,3-dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-one, 10.1 parts of sodium hydrogen carbonate and 160 parts of ethanol is stirred and refluxed overnight. The reaction mixture is cooled, filtered over hyflo and the filtrate is evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane, 10% of methanol and one drop of ammonium hydroxide, as eluent. The pure fractions are collected and the eluent is evaporated, yielding 4.4 parts of ethyl 2-[4-(2,3-dihydro-2-oxo-1H-benzimidazol-1-yl)-1-piperidinyl]ethylcarbamate as a residue.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04031226 |
| 出典データセット | uspto-grants-1977_06 |
| ORD ID | ord-73c8c05ebae646fc8d699fc2200a374d |
| 出典メモ | uspto-grants-1977_06 |