化工社化工社 化学情報印刷レポート · 研究参考用
Dimethylformamide → 1,4,6-Trimethyl-1H-indole-3-carbaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Diphosphoryl tetrachloride | HCID 4432411 | — |
| 反応物 | 1,4,6-Trimethyl-1H-indole | HCID 13411053 | — |
| 生成物 | 1,4,6-Trimethyl-1H-indole-3-carbaldehyde | HCID 53433946 | — |
反応手順
A solution of 1,4,6-trimethyl-1H-indole (800 mg, 5 mmol) in DMF (0.9 mL) was cooled to 5° C. under nitrogen. The pyrophosphoryl chloride (1.4 mL, 10 mmol) was then slowly introduced. Upon complete addition the cooling bath was removed and the reaction was allowed to warm to ambient temperature. After a total of 45 minutes the reaction was cooled to 5° C. and slowly quenched with 2N NaOH. The pH was adjusted to 8. The solid that precipitate out from the solution was collected by filtration and was washed with water. The remaining white solid was dried in the oven and was confirmed to be the title compound (875 mg, 93%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09062056B2 |
| 出典データセット | uspto-grants-2015_06 |
| ORD ID | ord-f6aa131a51cf4c0e9c7d24e49de30bef |
| 出典メモ | uspto-grants-2015_06 |