関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1-(2-Chlorobenzo[d]thiazol-5-yl)ethanone | HCID 21703643 | — |
| 反応物 | Potassium hydrogensulfide | HCID 86743134 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-(2-Thioxo-2,3-dihydrobenzo[d]thiazol-5-yl)ethanone | HCID 21703644 | 80.9% |
反応手順
A mixture of 5-acetyl-2-chlorobenzothiazole (137 mg, 0.65 mmol), potassium hydrogen sulfide (94 mg, 1.30 mmol) and ethanol (3.3 mL) in a capped flask was stirred in an oil bath at 80° C. for two hours. The mixture was cooled in ice, acidified with 1N hydrochloric acid (1.35 mL) and evaporated in vacuo. The residue was partitioned between water (25 mL) and ethyl acetate (50, 25 mL). The organic extracts were washed with brine, dried over magnesium sulfate, filtered and evaporated in vacuo to a solid (133 mg). This material was triturated with ether and dried to provide 5-acetyl-2-thioxo-2,3-dihydrobenzothiazole (110 mg) as a pale yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06288054B1 |
|---|
| 出典データセット | uspto-grants-2001_09 |
|---|
| ORD ID | ord-9b36e4436751483e9091064a182868fc |
|---|
| 出典メモ | uspto-grants-2001_09 |
|---|