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Chloroacetic Acid → 5-chloro-2-(chloromethyl)-1H-1,3-benzodiazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroacetic Acid | HCID 300 | — |
| 反応物 | 4-Chloro-1,2-diaminobenzene | HCID 7263 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | 5-chloro-2-(chloromethyl)-1H-1,3-benzodiazole | HCID 271286 | 69.4% |
反応手順
The solution of 4-chloro-1,2-phenylenediamine (1.43 g) and chloroacetic acid (1.43 g) in 4M HCl (10 ml) was heated to reflux for 1 h. After cooling to rt overnight the mixture was filtered and the filtrate was cooled in an ice bath. With stirring the solution was adjusted to pH 8 with 25% ammonia solution. A gummy precipitate is formed which is cooled for 1 h. The aqueous layer is removed by decantation and the residue crystallised from acetone/water to yield 5-chloro-2-chloromethylbenzimidazole (1.4 g) as brownish solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08912186B2 |
| 出典データセット | uspto-grants-2014_12 |
| ORD ID | ord-fb14993c22a241f48bb602afa6032bab |
| 出典メモ | uspto-grants-2014_12 |