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2-Propenoic acid, 2-azido-3-(3,4,5-trimethoxyphenyl)-, methyl ester → methyl 5,6,7-trimethoxy-1H-indole-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Propenoic acid, 2-azido-3-(3,4,5-trimethoxyphenyl)-, methyl ester | HCID 4306247 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | methyl 5,6,7-trimethoxy-1H-indole-2-carboxylate | HCID 4453649 | — |
反応手順
Xylene (15 mL) was placed in a three-necked flask and stirred under reflux, and a xylene solution (30 mL) of methyl 3-(3,4,5-trimethoxyphenyl)-2-azidopropenoate (1.2 g) was added dropwise over 3 hours. The reaction mixture was refluxed for 1 hour and concentrated under reduced pressure. Water was added to the residue to conduct extraction with ethyl acetate. The extract was washed with water and saturated brine, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (ethyl acetate:hexane 1:3) to obtain the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06632810B2 |
| 出典データセット | uspto-grants-2003_10 |
| ORD ID | ord-f2a2104971084473957f0ed4e35ffe2e |
| 出典メモ | uspto-grants-2003_10 |