化工社化工社 化学情報印刷レポート · 研究参考用
6-Fluoro-5-Hydroxy-4-Nitro-Hexanoic Acid Methylamide → 4-Amino-6-Fluoro-5-Hydroxy-Hexanoic Acid Methylamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 6-Fluoro-5-Hydroxy-4-Nitro-Hexanoic Acid Methylamide | HCID 86625110 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-Amino-6-Fluoro-5-Hydroxy-Hexanoic Acid Methylamide | HCID 86625111 | 90% |
反応手順
To a solution of 6-fluoro-5-hydroxy-4-nitro-hexanoic acid methylamide (0.325 g, 1.56 mmol) in MeOH (12 mL) was added Raney Ni (about 0.12 g), and the mixture was shaken under H2 (40-45 psi) at room temperature for 18 h. The black mixture was filtered through celite, and the celite was washed with additional MeOH (100 mL). The yellow solution was concentrated to give yellow oil (0.250 g, 90%), which was used without further purification. 1H NMR (CDCl3): 5.68 (br s, NH, 1H), 4.64-4.38 (m, 2H), 3.64-3.49 (m, 1H), 2.90-2.85 (m, 1H), 2.81 (d, J=5.10 Hz, 3H), 2.40-2.29 (m, 2H), 1.97-1.88 (m, 2H); Mass Spectra: ESI: calculated: 178.11. found: MH+ 179.18.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07504382B2 |
| 出典データセット | uspto-grants-2009_03 |
| ORD ID | ord-0b7d8e7f59b64f14b2c09fbad273ee7f |
| 出典メモ | uspto-grants-2009_03 |