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HRID 1791999作成日:2026年10月25日
1,8-Diazabicyclo(5.4.0)undec-7-ene → 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
https://huagongshe.com/reaction/1791999
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 反応物 | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| 反応物 | 7-Allyl-8-chloro-1,3-dimethyl-3,7-dihydropurine-2,6-dione | HCID 738682 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 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 | 94.4% |
反応手順
A mixture of 7-allyl-8-chloro-1,3-dimethyl-3,7-dihydropurine-2,6-dione (1.0 g), piperazine-1-carboxylic acid tert-butyl ester (1.1 g), 1,8-diazabicyclo[5,4,0]undec-7-ene (DBU) (0.59 ml), and 1-methylpyrrolidin-2-one (2 ml) were stirred under nitrogen atmosphere in an oil bath at 140° C. for 2 hours. The reaction mixture was extracted with ethyl acetate and water. The organic layer was washed with water followed by saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography with 10–20% (20% 2-propanol/ethyl acetate)/hexane to give 1.5 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07074798B2 |
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| 出典データセット | uspto-grants-2006_07 |
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| ORD ID | ord-c838971beba043dab0973b4dd0a71f71 |
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| 出典メモ | uspto-grants-2006_07 |
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