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Dimethylformamide dimethyl acetal → 3-(Dimethylaminomethyleneamino)benzofuran-2-carboxylic Acid Ethyl Ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| 反応物 | Ethyl 3-aminobenzofuran-2-carboxylate | HCID 2063537 | — |
| 生成物 | 3-(Dimethylaminomethyleneamino)benzofuran-2-carboxylic Acid Ethyl Ester | HCID 9834962 | 75% |
反応手順
A mixture of 4.2 g (20.0 mmol) of ethyl 3-amino-2-benzo[b]furancarboxylate (EP 187487 A1) in 10 mL of N,N-dimethylformamide dimethyl acetal is heated at reflux temperature for 1.5 hours, then cooled to room temperature and concentrated in vacuo. The residue is partitioned between ethyl acetate and water. The organic layer is washed with water, dried over sodium sulfate, passed through a pad of diatomaceous earth and concentrated in vacuo. The solid is collected by filtration to provide 3.90 g (75%) of a white solid, mp 89–90° C.;
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07105531B2 |
| 出典データセット | uspto-grants-2006_09 |
| ORD ID | ord-e6aec541f4d14e00ade674578fe2a4bb |
| 出典メモ | uspto-grants-2006_09 |