関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 5-Nitrovanillin | HCID 81134 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3,4-Dimethoxy-5-nitrobenzaldehyde | HCID 10867565 | — |
反応手順
A suspension of sodium hydride (4.87 g, 121.7 mmole) in 18 mL dry DMF was cooled to 0° C. and then 5-nitrovanillin (20 g, 101.4 mmole) in 30 mL of DMF was added dropwise. After 30 minutes, methyl iodide (43.18 g, 304.2 mmole) was added dropwise at 0° C. When the addition was completed, the mixture was warmed to room temperature and stirred overnight. Water was added and the solution extracted with ethyl ether, the organic layer was washed with 10% NaOH solution, dried over MgSO4, filtered and evaporated in vacuo to an oil (8.7 g, 40.7%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05856323 |
|---|
| 出典データセット | uspto-grants-1999_01 |
|---|
| ORD ID | ord-199b9efcfdb54d4e868c96008a8f708e |
|---|
| 出典メモ | uspto-grants-1999_01 |
|---|
