関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4,4-Dimethoxy-2-butanone | HCID 228548 | — |
| 反応物 | HCID 178509291 | HCID 178509291 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Benzylthio-7-methyl-1,2,4-triazolo[1,5-a]pyrimidine | HCID 14155087 | 43.9% |
反応手順
A solution of 50 g (0.24 mol) of 3-amino-5-benzylthio-1,2,4-triazole in 500 ml of glacial acetic acid was added dropwise over 3-4 hours to a solution of 34.0 g (0.25 mol) of acetylacetaldehyde dimethyl acetal in 500 ml of glacial acetic acid heated at 100° C. After the addition was complete the reaction mixture was heated at reflux overnight, cooled to room temperature and poured into an ice-water mixture. The solid which separated was collected by filtration and recrystallized from ethanol to yield 27 g (41%) of the desired product as a solid, m.p. 102°-104° C. IR and 1H NMR spectra were in agreement with the assigned structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04886883 |
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| 出典データセット | uspto-grants-1989_12 |
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| ORD ID | ord-05c353504bb1462c99a364cae839346e |
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| 出典メモ | uspto-grants-1989_12 |
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