関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethylcarbamoyl chloride | HCID 6916 | — |
| 反応物 | 1-(Hydroxymethyl)-4-propylpyrrolidin-2-one | HCID 11332602 | — |
| 反応物 | HCID 178478416 | HCID 178478416 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-[(6-chloro-9H-purin-9-yl)methyl]-4-propylpyrrolidin-2-one | HCID 57743009 | 99% |
反応手順
A mixture of 6-chloro-1H-purine x165 (2 g, 12.93 mmol, 1 eq), 1-(hydroxymethyl)-4-propylpyrrolidin-2-one x2 (2.44 g, 15.53 mmol, 1.2 eq) and N,N-diethylcarbamoylchloride (332 mg, 1.293 mmol, 0.1 eq) in MeCN (30 ml) is heated at 100° C. in microwave apparatus during 5 hours. After cooling, the solvent is evaporated and the crude is purified on silicagel (CH2Cl2/MeOH (+NH4OH 10%) 95/5) to yield 3.8 g of 1-[(6-chloro-9H-purin-9-yl)methyl]-4-propylpyrrolidin-2-one x166 as a pale yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08586623B2 |
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| 出典データセット | uspto-grants-2013_11 |
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| ORD ID | ord-9e50b3f5c0d1475c9f4f520cd26571f1 |
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| 出典メモ | uspto-grants-2013_11 |
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