関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,3-Dibromobutane | HCID 21508 | — |
| 反応物 | HCID 178481768 | HCID 178481768 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6,7-Dihydro-1,6,7-trimethylpyrazolo[3,4-d]thiazolo[3,2-a]pyrimidin-4(1H)-one | HCID 22401673 | 12.1% |
反応手順
In 200 ml of dimethylformamide was dissolved 10.0 g (54.9 mmol) of 4,5-dihydro-6-mercapto-1-methylpyrazolo[3,4-d]pyrimidin-4(1H)-one [Helv. Chim. Acta, 42, 349 (1959)], and 15.2 g (110 mmol) of potassium carbonate and 10.1 ml (82.3 mmol) of 2,3-dibromobutane were added to the solution, followed by stirring at 80° C. for 3 hours. After evaporation of the solvent, the residue was subjected to partition between chloroform and water, and the chloroform layer was concentrated to dryness under reduced pressure. The residue was subjected to silica gel column chromatography and eluted with chloroform to give 1.57 g (12%) of Compound 41. The compound was recrystallized from ethyl acetate/hexane for purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05527908 |
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| 出典データセット | uspto-grants-1996_06 |
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| ORD ID | ord-2f37cf315c344f1a8a4df1cb3158c984 |
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| 出典メモ | uspto-grants-1996_06 |
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