化工社化工社 化学情報印刷レポート · 研究参考用
Dimethyl-p-toluidine → 6,8-Dichloro-3-(5-cyclopropyl-[1,2,4]oxadiazol-3-yl)-4H-2,5,10b-triaza-benzo[e]azulene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethyl-p-toluidine | HCID 7471 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | HCID 22713497 | HCID 22713497 | — |
| 溶媒 | Chlorobenzene | HCID 7964 | — |
| 生成物 | 6,8-Dichloro-3-(5-cyclopropyl-[1,2,4]oxadiazol-3-yl)-4H-2,5,10b-triaza-benzo[e]azulene | HCID 22713545 | 63% |
反応手順
8-Chloro-3-(5-cyclopropyl-[1,2,4]oxadiazol-3-yl)-4,5-dihydro-2,5,10b-triaza-benzo[e]azulen-6-one (0.84 g, 2.5 mmol) was suspended in chlorobenzene (8 mL), N,N-dimethyl-p-toluidine (1.1 mL, 7.4 mmol) and phosphorus oxychloride (0.34 mL, 3.7 mmol) were added and the mixture was refluxed overnight. The resulting solution was evaporated and the residue was purified by chromatography on silica gel in CH2Cl2/acetone 10:1. One obtained a white solid (0.56 g, 63%). mp 200° C. m/z 359(M).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06743789B2 |
| 出典データセット | uspto-grants-2004_06 |
| ORD ID | ord-80f739d1ea654a9eb6c80e6283701e33 |
| 出典メモ | uspto-grants-2004_06 |