化工社化工社 化学情報印刷レポート · 研究参考用
Acetic Acid → Ethyl 2-(benzylsulfanyl)-7-methyl[1,2,4]triazolo[1,5-a]pyrimidine-6-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Ethyl ethoxymethyleneacetoacetate | HCID 54463595 | — |
| 反応物 | HCID 178509291 | HCID 178509291 | — |
| 生成物 | Ethyl 2-(benzylsulfanyl)-7-methyl[1,2,4]triazolo[1,5-a]pyrimidine-6-carboxylate | HCID 14155094 | 33% |
反応手順
A solution of 15 g (73 mmol) of 3-amino-5-benzylthio-1,2,4-triazole and 15.0 g (80.0 mmol) of ethyl ethoxymethyleneacetoacetate in 250 ml of glacial acetic acid was heated at reflux for 60 hours. After cooling the volume of the reaction was reduced to approximately one quarter of the oroginal volume by evaporation at reduced pressure. The resulting residue was poured into water, and the solid which separated was collected by filtration, washed with water and dried to yield 7.88 g (33%) of the desired product as a solid, m.p. 98°-99° 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 | US04740233 |
| 出典データセット | uspto-grants-1988_04 |
| ORD ID | ord-e1cd40e7dd7140279e3f66a84655481d |
| 出典メモ | uspto-grants-1988_04 |