化工社化工社 化学情報印刷レポート · 研究参考用
N,N-Dimethylaniline → 12-Chloro-7-thia-9,11-diazatricyclo(6.4.0.0,2,6)dodeca-1(12),2(6),8,10-tetraene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N,N-Dimethylaniline | HCID 949 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 5,6,7,8-Tetrahydro(1)benzothieno(2,3-D)pyrimidin-4(3H)-one | HCID 98614 | — |
| 生成物 | 12-Chloro-7-thia-9,11-diazatricyclo(6.4.0.0,2,6)dodeca-1(12),2(6),8,10-tetraene | HCID 789817 | — |
反応手順
To 10.56 g 5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidin-4(3H)-one (0.51 mol) and 10 mL dimethylaniline was added, in one portion, 50 mL POCl3. The mixture was heated to reflux for 5 h under argon, cooled and the excess POCl3 was removed by concentration in vacuo. The residue was poured into 200 g ice and neutralized with satd Na2CO3. The resulting blue-gray gum was filtered, washed with water and crystallized from ethanol to give 7.03 g (0.031 mol) of product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06849638B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-f8d24aee8efc4d0395001177f0ee1e21 |
| 出典メモ | uspto-grants-2005_02 |