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Acetonitrile → 5-[2-(4-(4-Phenoxyphenyl)piperidin-1-yl)acetylamino]-2,3,4,5-tetrahydro-1-benzoxepine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | 4-(4-Phenoxyphenyl)piperidine | HCID 11075984 | — |
| 反応物 | 5-(2-Bromoacetylamino)-2,3,4,5-tetrahydro-1-benzoxepine | HCID 19694270 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | 5-[2-(4-(4-Phenoxyphenyl)piperidin-1-yl)acetylamino]-2,3,4,5-tetrahydro-1-benzoxepine | HCID 19694253 | 98% |
反応手順
To a 5 ml acetonitrile solution of 190 mg of the compound (8) synthesized in Reference Example 8 were added 184 mg of the compound (4) synthesized in Reference Example 4 and 0.14 ml of triethylamine. This was heated at reflux for 3 hours. To the reaction was added 10 ml of ice water, then extraction was performed with ethyl acetate. The extract was dried, filtered, then concentrated under reduced pressure to obtain a residue which was then purified by silica gel column chromatography (methylene chloride:methanol=25:1) to obtain the above-identified compound (28) in an amount of 300 mg (yield of 98%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05723475 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-23b3904cefa54993927e4b9f165740eb |
| 出典メモ | uspto-grants-1998_03 |