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Ethyl alpha-Azido-beta-(4-methoxypyrid-3-yl)-acrylate → Ethyl 4-methoxy-1H-pyrrolo[2,3-b]pyridine-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl alpha-Azido-beta-(4-methoxypyrid-3-yl)-acrylate | HCID 72796408 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | Ethyl 4-methoxy-1H-pyrrolo[2,3-b]pyridine-2-carboxylate | HCID 11736140 | — |
反応手順
A stirred solution of ethyl-α-azido-β-(4-methoxypyrid-3-yl)-acrylate 2 (3.7 g, 14.9 mmol) in dry o-xylene (35 mL) was heated in an oil bath at 170° C. for 25 min. During this time the contents of the flask gained brick red color. After cooling, the mixture was concentrated under high vacuum. The resultant brown residue was purified on silica gel column using 5% methanol in CH2Cl2 to give 3 as brick red solid. Mp 195-197° C.; Yield: 3.3 g, 82%; ESI MS: m/z 220.9 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07666898B2 |
| 出典データセット | uspto-grants-2010_02 |
| ORD ID | ord-1feb00a08af34c57a4e5d752862b7d45 |
| 出典メモ | uspto-grants-2010_02 |