関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | 1,3-Dicyclopropylmethyl xanthine | HCID 15291303 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 1,3-Dicyclopropylmethyl-8-nitro xanthine | HCID 9857658 | 56.5% |
反応手順
1,3-Di-cyclopropylmethyl xanthine (20 g, 0,076 mol) was dissolved in acetic acid (33 ml) and then treated with concentrated nitric acid (13.2 g) at 87° C. After 1 hour, the mixture was cooled to 5° C. and the resulting yellow precipitate filtered off. The yellow crystals were dissolved in dichloromethane and washed with water. The separated organic layer was then dried over anhydrous sodium sulphate and concentrated in vacuo. The product crystallized from the concentrate to yield a yellow crystalline product yield 12.2 g, (56.5%), m.pt. 207° C. (with decomposition).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05734051 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-f3bd66fd965f4b3c8102b0b4627404bb |
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| 出典メモ | uspto-grants-1998_03 |
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