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Triethylamine → rac-[(5-Chloro-1,3-benzothiazol-2-yl)thio](phenyl)acetic Acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Bromo(phenyl)acetic acid | HCID 97919 | — |
| 反応物 | HCID 178527796 | HCID 178527796 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | rac-[(5-Chloro-1,3-benzothiazol-2-yl)thio](phenyl)acetic Acid | HCID 12928398 | 70% |
反応手順
To a solution of 5-chloro-2-mercaptobenzothiazole (38 g, 0.188 mol) in methylene chloride (750 mL) was added α-bromophenylacetic acid (38 g, 0.177 L mol) and triethylamine (38.5 g, 53 mL, 0.38 mol). The mixture was heated to reflux overnight. The clear solution was evaporated in vacuo and the residue was taken up in ethyl acetate, washed with dilute hydrochloric acid solution, then with water and finally dried over magnesium sulfate and filtered. The filtrate was concentrated in vacuo to a small volume and treated with n-hexane whereby the product crystallized out. Filtration yielded the product as a beige crystalline compound (41 g, 70%), m.p. 184°-185° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04866082 |
| 出典データセット | uspto-grants-1989_09 |
| ORD ID | ord-d0a985991e584ee596db388be46e5347 |
| 出典メモ | uspto-grants-1989_09 |