化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 3-(Benzo-1,2,3-thiadiazole-7-carbonyloxy)-5,5-dimethyl-cyclohex-2-enone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Dimedone | HCID 31358 | — |
| 反応物 | 1,2,3-Benzothiadiazole-7-carbonyl chloride | HCID 18377607 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-(Benzo-1,2,3-thiadiazole-7-carbonyloxy)-5,5-dimethyl-cyclohex-2-enone | HCID 19793418 | 87.5% |
反応手順
5.6 g (0.04 mol) of 5,5-dimethyl-1,3-cyclohexanedione are dissolved in a mixture of 4.4 g (0.044 mol) of triethylamine and 120 ml of ethyl acetate. 8.7 g (0.044 mol) of benzothiadiazole-7-carboxylic acid chloride are added dropwise at 15° to 20° C., and the mixture is subsequently stirred overnight at room temperature. The ethyl acetate solution is washed with H2O, dried and concentrated. Purification by column chromatography using ethyl acetate/hexane gives 10.5 g (87.5%) of the title compound, melting point 131°-133° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05248683 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-8e967b2fdeb8454a83c24e9d3bcde951 |
| 出典メモ | uspto-grants-1993_09 |