化工社化工社 化学情報印刷レポート · 研究参考用
Methyl iodide → 1-Methyl-6-methylsulfonyl-indole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 6-methanesulfonyl-1H-indole | HCID 2761067 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 生成物 | 1-Methyl-6-methylsulfonyl-indole | HCID 67305770 | — |
反応手順
To a slurry of sodium hydride (60% in mineral oil, 0.90 g, 23 mmol) was added in portions 6-(methylsulfonyl)-1H-indole (4.0 g, 20 mmol) over 5 minutes at 5-10° C. The reaction mixture was stirred at rt for 1 h until hydrogen evolution ceased, and methyl iodide was added dropwise over 5 minutes at 10-20° C. The mixture was stirred at rt for 1 h, quenched with ice/water, and extracted with tert-butylmethyl ether. The organics were washed, dried and concentrated. The residue was crystallized from ether/hexane to yield the desired compound (3.8 g) as a yellowish solid. MS (ISP): m/e 210.1 (M+H)+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07973051B2 |
| 出典データセット | uspto-grants-2011_07 |
| ORD ID | ord-9d5b83a1bc4549048bad5a5140fbae72 |
| 出典メモ | uspto-grants-2011_07 |