関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Quinoline | HCID 7047 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 反応物 | HCID 178418609 | HCID 178418609 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | HCID 178418674 | HCID 178418674 | — |
反応手順
A mixture of 2 g of 3-(3-tetrahydropyr-2-yloxyprop-1-yn-1-yl)-4-hydroxy-6-pivaloylaminopyrrolo[2,3-d]pyrimidine, 40 ml of methanol, 20 ml of chloroform, 40 mg of 5% palladium on barium sulfate, and 40 mg of synthetic quinoline is stirred under 1 atmosphere hydrogen pressure for 40 min. The solvent then is removed by evaporation and the residue diluted with methylene chloride. The methylene chloride solution is filtered through silica gel with 2% methanol in methylene chloride to remove catalyst and the filtrate then concentrated to give an oil which upon adding ether yields 3-(3-tetrahydropyr-2-yloxyprop-1-en-1-yl)-4-hydroxy-6-pivaloylaminopyrrolo[2,3-d]pyrimidine which can be further purified through column chromatography eluting with ethyl acetate and recrystallization using ethyl acetate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05248775 |
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| 出典データセット | uspto-grants-1993_09 |
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| ORD ID | ord-68835ea9559e4264a057fa5856eb6da6 |
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| 出典メモ | uspto-grants-1993_09 |
|---|