化工社化工社 化学情報印刷レポート · 研究参考用
Ethanol → 2,3,8,9-Tetrahydro-5-(4-methoxy-2,3-dimethylphenyl)-9-[(4-methoxy-2,3-dimethylphenyl)-methylene]-5H,6H-pyrano[4,3-d]thiazolo[3,2-a]pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | 4,5-Dihydro-2-thiazolamine | HCID 15689 | — |
| 反応物 | Tetrahydro-3,5-bis[(4-methoxy-2,3-dimethylphenyl)methylene]-4H-pyran-4-one | HCID 54006504 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2,3,8,9-Tetrahydro-5-(4-methoxy-2,3-dimethylphenyl)-9-[(4-methoxy-2,3-dimethylphenyl)-methylene]-5H,6H-pyrano[4,3-d]thiazolo[3,2-a]pyrimidine | HCID 21786681 | 74.5% |
反応手順
A stirred solution of tetrahydro-3,5-bis[(4-methoxy-2,3-dimethylphenyl)methylene]-4H-pyran-4-one (3.0 g, 7.6 mmole) and 2-amino-2-thiazoline (1.0 g, 9.7 mmole) in 75 ml of CHCl3 is heated at reflux temperature for 72 hours. After cooling, the solution is filtered to remove a small amount of insoluble material. The solvent is evaporated to give an oily residue. Trituration with warm EtOH yields 2.7 g of a yellow solid, m.p. 226°-228° d. Crystallization from 15 ml of DMF gives 2.3 g (63%) of cream colored product, m.p. 235°-237°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04128648 |
| 出典データセット | uspto-grants-1978_12 |
| ORD ID | ord-0216767bb51d4822929f14d5e9fea3a9 |
| 出典メモ | uspto-grants-1978_12 |