化工社化工社 化学情報印刷レポート · 研究参考用
Sodium borohydride → HCID 178518613、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | 3-(4-Fluorophenyl)propan-1-amine | HCID 6483796 | — |
| 反応物 | 6-(4-oxocyclohexyl)-3H-benzothiazol-2-one | HCID 22669109 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | HCID 178518613 | HCID 178518613 | 7% |
反応手順
To a solution of ketone 25 (2.3 g, 9.3 mmol) in 2-propanol (30 mL) was added 4 Å molecular sieves and 3-(4-fluorophenyl)-1-propylamine (1.76 g, 9.3 mmol). The reaction mixture was stirred for 4 hours. Sodium borohydride (0.49 g, 13.03 mmol) was added, and the reaction mixture was stirred overnight, quenched with MeOH, and concentrated under reduced pressure. Purification by flash chromatography (silica, 9.5:5:1 CH2Cl2:MeOH:NH4OH) gave 6-{trans-4-[3-(4-fluorophenyl)propylamino]cyclohexyl}-3H-benzthiazol-2-one (0.24 g, 7%): 1H NMR (500 MHz, DMSO-d6): δ 7.39 (s, 1H), 7.25-7.06 (m, 6H), 3.01 (m, 1H), 2.86 (t, J=8 Hz, 2H), 2.61 (t, J=8 Hz, 2H), 2.37 (m, 1H), 2.01 (m, 2H), 1.92-1.81 (m, 4H), 1.49-1.36 (m, 4H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06794402B2 |
| 出典データセット | uspto-grants-2004_09 |
| ORD ID | ord-38016c99bab84550bd3cf33a66b347a3 |
| 出典メモ | uspto-grants-2004_09 |