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Trifluoroacetic acid → 7-Allyl-1,3-dimethyl-8-(piperazin-1-yl)-3,7-dihydropurine-2,6-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | 4-(7-Allyl-1,3-dimethyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl)piperazine-1-carboxylic acid tert-butyl ester | HCID 23536953 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 7-Allyl-1,3-dimethyl-8-(piperazin-1-yl)-3,7-dihydropurine-2,6-dione | HCID 22029967 | 66.4% |
反応手順
A mixture of 4-(7-allyl-1,3-dimethyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl)piperazine-1-carboxylic acid tert-butyl ester (1.5 g), trifluoroacetic acid (3 ml), and dichloromethane (10 ml) was stirred at room temperature for 3 hours. The reaction solution was concentrated under reduced pressure. Water (10 ml) and 5 M potassium carbonate aqueous solution (5 ml) were added to the residue, extracted with dichloromethane, then the organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was recrystallized from ethyl acetate-hexane to give 750 mg of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07074798B2 |
| 出典データセット | uspto-grants-2006_07 |
| ORD ID | ord-dd12a9129b4f4a8e9d7fbb561dade17d |
| 出典メモ | uspto-grants-2006_07 |