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Isobutyl chloroformate → 2-[(8-chlorodibenz[b,f][1,4]oxazepin-10(11H)-yl)carbonyl]-N-(4-pyridinylmethyl)benzamide, hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Isobutyl chloroformate | HCID 62365 | — |
| 反応物 | 4-Pyridinemethanamine | HCID 77317 | — |
| 反応物 | 2-[(8-chlorodibenz[b,f][1,4]oxazepin-10(11H)-yl)carbonyl]benzoic acid | HCID 15780657 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-[(8-chlorodibenz[b,f][1,4]oxazepin-10(11H)-yl)carbonyl]-N-(4-pyridinylmethyl)benzamide, hydrochloride | HCID 131719013 | — |
反応手順
To a stirred solution of the title product of Example 11 (0.55 g) in CH2Cl2 (10 mL) at 0° C. was added 1-methyl morpholine (0.168 mL) and isobutylchloroformate (0.199 mL) successively. After 30 minutes, 4-(aminomethyl)pyridine (0.156 mL) was added. The mixture was allowed to warm to ambient temperature for hours. The mixture was extracted with ethyl acetate and water. The organic extract was dried over MgSO4 and concentrated. The residue was purified by chromatography over silica gel using ethyl acetate as eluant to give the free base of the title compound as a white solid. The hydrochloride salt of the free base was made in the manner described in Example 3 to give the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05420270 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-5cbc34ffa9f54a88b61082ab7fa8a56e |
| 出典メモ | uspto-grants-1995_05 |