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Sodium → 2-Benzylthio-5,6-dimethyl-1,2,4-triazolo[1,5-a]pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | Butanal, 2-methyl-3-oxo- | HCID 11051586 | — |
| 反応物 | HCID 178509291 | HCID 178509291 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Benzylthio-5,6-dimethyl-1,2,4-triazolo[1,5-a]pyrimidine | HCID 14155092 | 54% |
反応手順
A solution of 5.0 g (24 mmol) of 3-amino-5-benzylthio-1,2,4-triazole and 5.0 g (41 mmol) of the sodium salt of 2-methyl-3-oxobutanal in 200 ml of glacial acetic acid was heated at reflux overnight. The solution was cooled to room temperature and the reaction mixture was concentrated by evaporation at reduced pressure. The residue was combined with ice and H2O to separate a tan solid. The solid was collected by filtration, dried and carefully recrystallized from ethyl acetate to yield 3.53 g (54%) of the desired product as a crystalline solid, m.p. 147°-149° 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 |
|---|---|
| 特許番号 | US04886883 |
| 出典データセット | uspto-grants-1989_12 |
| ORD ID | ord-d3cc2949956845dba26dd21283252a72 |
| 出典メモ | uspto-grants-1989_12 |