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4-Pyridineacetic acid hydrochloride → HCID 18780247、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Pyridineacetic acid hydrochloride | HCID 81097 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 18780247 | HCID 18780247 | 21.5% |
反応手順
5 g of 4-pyridyl-acetic acid hydrochloride and 3.72 g of diisopropylethylamine in 50 ml of dichloromethane were treated at 0° C. firstly with 6.37 g of 1-methylindole-3-glyoxylyl chloride in 50 ml of dichloromethane and then with 7.5 g of diisopropylethylamine. The mixture was allowed to warm to room temperature and was then stirred for 65 hours. The solvent was removed under reduced pressure and the residue was taken up in dichloromethane and chromatographed on silica gel with ethyl acetate. The product-containing fractions were concentrated. Crystallization from ethyl acetate/hexane yielded 940 mg of 3-(1-methyl-3-indolyl)-4-(4-pyridyl)furan-2,5-dione, m.p. 217°-219° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05057614 |
| 出典データセット | uspto-grants-1991_10 |
| ORD ID | ord-cefa521c988b459f8532c75ce1a6145a |
| 出典メモ | uspto-grants-1991_10 |