関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,1-Dichloroethane | HCID 6365 | — |
| 反応物 | Trimethylsilyl chlorosulphate | HCID 78059 | — |
| 反応物 | 7-chloro-1H-indole | HCID 104644 | — |
| 生成物 | 5-chloro-1H-indole-3-sulfonic acid | HCID 22574052 | — |
反応手順
7-Chloroindole (1.51 g, 10 mmole) was dissolved in 2 ml dichloroethane and cooled under nitrogen to −10° C. in an ice-salt-acetone bath. Trimethylsilylchlorosulfonate (1.89 g, 1.6 ml, 10 mmole) was slowly added with stirring. Upon termination of the addition, the reaction was allowed to warm to room temperature and stirred for 30 min at this temperature. The dark red solution was evaporated to dryness and the solvent was replaced with 50 ml ethyl acetate. Methanol (5 ml) was added and the solvents were removed and the residue thoroughly dried to afford the crude 5-chloro-1H-indole-3-sulfonic acid as a red oil. Step 2 7-Chloro-1H-indole-3-sulfonic acid dimethylamide
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06852726B2 |
|---|
| 出典データセット | uspto-grants-2005_02 |
|---|
| ORD ID | ord-70c1fae9fcc645429cb95f1019463575 |
|---|
| 出典メモ | uspto-grants-2005_02 |
|---|