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3-Chloro-2,4-pentanedione → 2-Benzylthio-6-chloro-5,7-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 | 3-Chloro-2,4-pentanedione | HCID 74328 | — |
| 反応物 | HCID 178509291 | HCID 178509291 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Benzylthio-6-chloro-5,7-dimethyl-1,2,4-triazolo[1,5-a]pyrimidine | HCID 14155089 | 79% |
反応手順
To a suspension of 153 g (0.74 mol) 3-amino-5-benzylthio-1,2,4-triazole in 250 ml of glacial acetic acid was added to 100 g (0.74 mol) of 3-chloro-2,4-pentanedione in a dropwise manner. The reaction mixture was heated at reflux for 18 hours and cooled to room temperature. The reaction mixture was poured over ice and the oil which separated solidified upon stirring. The solid was collected by filtration and recrystallized from methanol to yield 116 g (79%) of the desired product as an off white solid, m.p. 164°-166° 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 | US04755212 |
| 出典データセット | uspto-grants-1988_07 |
| ORD ID | ord-8683b7b20f264843a3ed68f874477bb6 |
| 出典メモ | uspto-grants-1988_07 |