関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | HCID 178498586 | HCID 178498586 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 178519774 | HCID 178519774 | 91.9% |
反応手順
In 4 liters of ethanol was suspended 48.94 g of 7-hydroxy-2-hydroxymethyl-5-methoxycarbonyl-s-triazolo[1,5-a]pyrimidine, and 33 g of sodium borohydride was added little by little thereto and then the mixture was stirred at room temperature for 3 hours and then refluxed for 4 hours. A residue obtained by removing ethanol was dissolved in 2 liters of water, and 500 ml of Amberlite IRC-50 (H+) (trade name) was added thereto and stirred. Subsequently, the mixture was filtered and after removing water from the filtrate, 500 ml of methanol was added to the filtrate and the mixture was stirred. Then, methanol was removed from the mixture to obtain a residue. These procedures were repeated three times. Then, 500 ml of ethanol was added to the residue and the mixture was condensed. Precipitated crystal was collected by filtration, washed with ethanol and dried to obtain 39.35 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 | US04987129 |
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| 出典データセット | uspto-grants-1991_01 |
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| ORD ID | ord-0b3794cb1b4f4730a851113d9b1fc5b4 |
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| 出典メモ | uspto-grants-1991_01 |
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