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(S)-2-[(azepane-1-carbonyl)-amino]-4-methyl-pentanoic acid benzyl ester → (2S)-2-(azepane-1-carbonylamino)-4-methylpentanoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | (S)-2-[(azepane-1-carbonyl)-amino]-4-methyl-pentanoic acid benzyl ester | HCID 10593708 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (2S)-2-(azepane-1-carbonylamino)-4-methylpentanoic acid | HCID 7530182 | 93.5% |
反応手順
A solution of (S)-2-[(azepane-1-carbonyl)-amino]-4-methyl-pentanoic acid benzyl ester (38.5 g, 111 mmol) in 600 mL of THF was hydrogenated at 50 psi over 20% Pd/C (2.00 g) for 17 minutes. The reaction mixture was filtered through celite and concentrated to dryness. The residue was heated in 50 mL of hexane. The resulting suspension was cooled, and the solid was collected by filtration and washed with hexane. The solid was dried at room temperature under vacuum to give (S)-2-[(azepane-1-carbonyl)-amino]-4-methyl-pentanoic acid as a white solid (26.6 g, 93%); mp 88-89° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06362174B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-bcbd6ef11e20417ca0c846e11fb335bc |
| 出典メモ | uspto-grants-2002_03 |