関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Fluoro-1,3-dimethyl-5-nitrobenzene | HCID 11367232 | — |
| 反応物 | 3-isopropyl-1H-indol-5-ol | HCID 22669491 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Isopropyl-5-(4-nitro-2,6-dimethyl-phenoxy)-1H-indole | HCID 22669511 | — |
反応手順
11.44 g (58.76 mmol) of 5-hydroxy-3-isopropyl-indole are dissolved in 350 ml of DMSO, 8.93 g (64.63 mmol) of potassium carbonate in solid form are introduced and subsequently 9.94 g (58.76 mmol) of 3,5-dimethyl-4-fluoronitrobenzene are added. The reaction solution is stirred for 2 hours at 100° C. under argon. Afterwards it is cooled to room temperature, 100 ml of ethyl acetate and 600 ml of H2O are added; ethyl acetate is separated off after phase separation and the aqueous phase is reextracted twice with ethyl acetate. The combined organic phases are washed twice with sodium chloride solution, dried over sodium sulphate, filtered and concentrated to dryness. The residue is purified by chromatography on silica gel by means of cyclohexane/ethyl acetate (10:1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06794406B2 |
|---|
| 出典データセット | uspto-grants-2004_09 |
|---|
| ORD ID | ord-c65647b50728423e988ab1d275144b03 |
|---|
| 出典メモ | uspto-grants-2004_09 |
|---|