関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formamidine acetate | HCID 160693 | — |
| 反応物 | 4,5-Diamino-3-chloro-2-phenylamino-benzoic acid methyl ester | HCID 85868198 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 7-Chloro-6-phenylamino-3H-benzoimidazole-5-carboxylic acid methyl ester | HCID 86599017 | 100.3% |
反応手順
4,5-Diamino-3-chloro-2-phenylamino-benzoic acid methyl ester 6b (0.32 g, 1.09 mmol) and formamidine acetate (72 mg, 1.64 mmol) in EtOH (36 mL) are heated, with stirring, to 80° C. After 44 hours, the reaction mixture is cooled to room temperature and diluted with EtOAc and washed with water (3×), saturated NaHCO3, and brine. The combined organic extracts are dried (Na2SO4) and concentrated under reduced pressure to give 0.33 g (99%) clean desired product as a solid. MS APCI (+) m/z 302.3 (M+1) detected.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07425637B2 |
|---|
| 出典データセット | uspto-grants-2008_09 |
|---|
| ORD ID | ord-f81764e602c5428f9da52d9dfb3b0aa3 |
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| 出典メモ | uspto-grants-2008_09 |
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