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(S)-3-methoxymethylamino-1-(2-thienyl)propan-1-ol → 3-(N-Methylamino)-1-(2-thienyl)-1-propanol, (-)-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | (S)-3-methoxymethylamino-1-(2-thienyl)propan-1-ol | HCID 66769498 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-(N-Methylamino)-1-(2-thienyl)-1-propanol, (-)- | HCID 10095047 | — |
反応手順
(S)-3-methoxymethylamino-1-(2-thienyl)propan-1-ol obtained from Example 2 was dissolved in 10 ml of methanol with 8 mg of Raney-nickel. This resulting solution was provided in a glass autoclave and hydrogenated at 50° C. for 12 hours. Upon completion of hydrogenation, the reaction mixture was filtered, and the solvent was removed under reduced pressure to give a crystal compound (122 mg, 90.8% measured by HPLC assay, 95% ee). The crude product was further purified by re-crystallization in toluene to give a product with optical purity as high as 100% ee.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08530674B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-537cec39ad074689b915daafa307d603 |
| 出典メモ | uspto-grants-2013_09 |