関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethane, 2-bromo-1,1-diethoxy- | HCID 74852 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | HCID 178507952 | HCID 178507952 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178508865 | HCID 178508865 | 79% |
反応手順
A mixture of 136.7 g of bromoacetaldehyde diethylacetal, 347 mL of water, and 17.3 mL of concentrated HCl was heated to about 90° C. with vigorous stirring for about 30 minutes, at which time a clear solution was obtained. The solution was cooled to ambient temperature and 68.3 g of sodium acetate was added. The resulting solution was added, with stirring, to a suspension of 100 g of 2,4-diamino-6-hydroxypyrimidine and 34.2 g of sodium acetate in 739 mL of water, which had been heated to 70°-85° C. The reaction was allowed to proceed for 2 hours at 70°-85° C., at which time the reaction was complete. The mixture was cooled to 0° C. and stirred for about 1.5 hours. The mixture was then filtered and the collected product was washed with 500 mL of water and 500 mL of acetone, and dried, affording 72.3 g (79%) of 2-amino-4 -hydroxy-7H-pyrrolo[2,3-d]pyrimidine, mp>300° C. NMR δ6.03 (s, 2H), 6.13 (m, 1H), 6.56 (dd, J=3.3, 2.3 Hz, 1H), 10.23 (br s, 1H), 10.93 (br s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05426187 |
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| 出典データセット | uspto-grants-1995_06 |
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| ORD ID | ord-dfede456fd9e4c148ee79d0562641559 |
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| 出典メモ | uspto-grants-1995_06 |
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