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O-Phenylenediamine → 2-(1H-Benzimidazol-2-yl)-1,3-benzothiazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | O-Phenylenediamine | HCID 7243 | — |
| 反応物 | 2-Methylbenzothiazole | HCID 8446 | — |
| 反応物 | Sulfur | HCID 5362487 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | 2-(1H-Benzimidazol-2-yl)-1,3-benzothiazole | HCID 373878 | 13.7% |
反応手順
The heterogeneous mixture consisting of methylbenzothiazole (59.6 g, 0.4 mol), ortho-phenylenediamine (43.2 g, 0.4 mol) and sulfur (38.4 g, 1.2 mol) in 300 ml of pyridine was heated at the reflux point of pyridine for 22 hours. The reaction mixture was cooled and poured into a solution of brine. After extraction with ethyl acetate, washing of the organic phase 3 times with water, drying over sodium sulfate and concentration of the solvent under vacuum, the solid obtained was washed with acetone. After drying, 2-(1H-benzimidazol-2-yl)benzothiazole (13.8 g, yield: 13%) was obtained in the form of a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06221343B1 |
| 出典データセット | uspto-grants-2001_04 |
| ORD ID | ord-2d6cc20732844b04a3fbfb1784cb370e |
| 出典メモ | uspto-grants-2001_04 |