化工社化工社 化学情報印刷レポート · 研究参考用
Water → HCID 57493916、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2,5-Hexanedione | HCID 8035 | — |
| 反応物 | 2-Benzothiazolamine, 6-bromo- | HCID 85149 | — |
| 反応物 | Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) | HCID 466102 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | HCID 57493916 | HCID 57493916 | 84% |
反応手順
A solution 6-bromobenzo[d]thiazol-2-amine (5.75 g, 25.1 mmol), hexane-2,5-dione (2.95 mL, 25.1 mmol), and PPTS (0.95 g, 3.76 mmol) in benzene (100 ml) was refluxed for 16 h while water was removed with a Dean-Stark trap. The cooled mixture was poured into EtOAc (100 mL) and extracted with saturated aq. NaHCO3 (2×100 mL) and brine. The organic layer was dried over Na2SO4, filtered and concentrated in vacuo. The crude product was purified by column chromatography on silica gel using 9:1 EtOAc:hexanes as the eluent to give the title compound as an orange oil (6.46 g, 84%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09095590B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-820f38f64ed24e64920365a25f92ae34 |
| 出典メモ | uspto-grants-2015_08 |