化工社化工社 化学情報印刷レポート · 研究参考用
Ammonium Hydroxide → 3-(3-Aminomethyl-phenyl)-2-methyl-propionic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | 3-(3-Cyano-phenyl)-2-methyl-propionic acid methyl ester | HCID 54523024 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Ammonium Hydroxide | HCID 14923 | — |
| 生成物 | 3-(3-Aminomethyl-phenyl)-2-methyl-propionic acid methyl ester | HCID 53702591 | 144.7% |
反応手順
A mixture of 3-(3-cyano-phenyl)-2-methyl-propionic acid methyl ester of Step B (62 mg, 0.30 mmol) and palladium on carbon (10%, 50 mg) in MeOH (10 mL), EtOAc (10 mL), and ammonium hydroxide (5 mL) was hydrogenated at 40 psi for 24 h. The catalyst was removed via filtration through Celite with the aid of MeOH. The solvent was removed in vacuo. Chromatography (1:1 hexanes:EtOAc to CH2Cl2:MeOH:NH4OH, 95:5:0.1) provided the title compound of Step C (45 mg). 1H NMR (400 MHz, CD3OD) δ 7.31-7.14 (m, 4H), 3.94 (s, 2H), 3.59 (s, 3H), 2.96 (m, 1H), 2.72 (m, 2H), 1.12 (d, 3H); MS 208 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07442702B2 |
| 出典データセット | uspto-grants-2008_10 |
| ORD ID | ord-120b5c5a44184a788669a7139fadc03c |
| 出典メモ | uspto-grants-2008_10 |