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Acetic Acid → 3,3-Dimethyl-1-{2-[4-(7-fluoroindol-3-yl)-1-piperidinyl]-1-ethyl)-1,3-dihydro-2H-indol-2-one Monohydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 3,3-Dimethyl-1-{2-[4-(7-fluoroindol-3-yl)-1,2,5,6-tetrahydro-1-pyridyl]-1-ethyl}-1,3-dihydro-2H-indol-2-one | HCID 9865888 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Platinum oxide charcoal | HCID 57448742 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3,3-Dimethyl-1-{2-[4-(7-fluoroindol-3-yl)-1-piperidinyl]-1-ethyl)-1,3-dihydro-2H-indol-2-one Monohydrochloride | HCID 70286581 | — |
反応手順
3,3-Dimethyl-1-{2-[4-(7-fluoroindol-3-yl)-1,2,5,6-tetrahydro-1-pyridyl]-1-ethyl}-1,3-dihydro-2H-indol-2-one (0.6 g, 1.36 mmol) dissolved in ethanol (40 mls) and acetic acid (4 mls) was added to 10% platinum oxide/charcoal. Hydrogen was admitted for 12 h at 60 psi the catalyst was then removed by filtration, the catalyst washed with ethanol (3×75 mls), concentrated in vacuo and the resulting oil purified by column chromatography on silica with ethyl acetate/Hexane. The fractions containing product were collected and the solvent evaporated in vacuo to give a solid which was converted to the hydrochloride, which was subsequently dried in vacuo to give a solid, mp 172-174° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06166040 |
| 出典データセット | uspto-grants-2000_12 |
| ORD ID | ord-edf40b8c8d0543f4a2845dfa140ee7b7 |
| 出典メモ | uspto-grants-2000_12 |