関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Benzyl mercaptan | HCID 7509 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Chloro-3-nitropyridine | HCID 79613 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(Benzylthio)-3-nitropyridine | HCID 507300 | 85% |
反応手順
Ethanol (150 mL) was added to a mixture of 2-chloro-3-nitro-pyridine (5 g, 31.54 mmol) and potassium carbonate (4.8 g, 34.7 mmol). Benzyl mercaptan (4.09 mL, 34.7 mmol) was added followed by water (30 mL). The mixture stirred at 25° C. for 4 h. Water (350 mL) was added and the product precipitated. The solid was collected by vacuum filtration, rinsed with water (100 mL) and dried in vacuo for 4 h to afford the desired product, 2-benzylsulfanyl-3-nitro-pyridine (6.6 g, 26.8 mmol, 85%), as a yellow powder. 1H NMR (400 MHz, DMSO-d6) δ: 4.47 (2H, s), 7.21-7.31 (3H, m), 7.40-7.45 (3H, m), 8.58 (1H, dd, J1=8.6 Hz, J2=1.7 Hz), 8.83 (1H, dd, J1=4.7 Hz, J2=1.7 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08101800B2 |
|---|
| 出典データセット | uspto-grants-2012_01 |
|---|
| ORD ID | ord-a83dfb074b564b2195c64ef100a22449 |
|---|
| 出典メモ | uspto-grants-2012_01 |
|---|