関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,2-Phenylenediamine dihydrochloride | HCID 11990 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Cyclopropanecarboxylic acid | HCID 15655 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-cyclopropyl-1H-1,3-benzodiazole | HCID 1084419 | 13% |
反応手順
2-cyclopropanecarboxylic acid (4 g, 52 mmol) was treated with phenylenediamine bis-hydrochloride (1 eq) and polyphosphosphoric acid (52 mL) and heated to 160° C. for 6 h. The reaction was cooled to 0° C. and diluted with water, then basified with NaOH (50% aqueous) until pH>10. The solution was extracted with ethyl acetate, dried (MgSO4), filtered and concentrated, purified by flash chromatography (100% ethyl acetate) giving 2-cyclopropylbenzimidazole (1.1 g, 13%). MS found: (M+H)+=159.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06720329B2 |
|---|
| 出典データセット | uspto-grants-2004_04 |
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| ORD ID | ord-6ebfa19a6cfc4642af8e40307979b7b3 |
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| 出典メモ | uspto-grants-2004_04 |
|---|
