関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-(4-(2-Propyloxyethoxy)benzoyl)-2-methylindole-4-acetic Acid | HCID 21974383 | — |
| 反応物 | HCID 178418416 | HCID 178418416 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | methyl 2-methyl-1H-indole-4-carboxylate | HCID 11769304 | — |
反応手順
To a solution of 2-methyl-4-trifluoromethanesulfoxyindole (6.32 g; prepared in Reference Example 1) in methanol (33.43 ml)-N,N-dimethylformamide (200 ml) was added triethylamine (6.3 ml) and tetrakis(triphenylphosphine)palladium (2.6 g). The inside of the vessel was replaced with carbon monoxide and the mixture was stirred at 60° C. overnight. After the reaction was completed, to the mixture was added water and ethyl acetate and then the mixture was extracted. The aqueous layer was extracted with ethyl acetate. The combined organic layer was washed with water and a saturated aqueous solution of sodium chloride, successively, dried and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (n-hexane-ethyl acetate) to give the title compound (4.29 g) having the following physical data.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07098234B2 |
|---|
| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-0da4b96c7f31489a97331b969fe85f03 |
|---|
| 出典メモ | uspto-grants-2006_08 |
|---|
