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Methyl 2,2,2-trichloroacetimidate → HCID 178497356、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl 2,2,2-trichloroacetimidate | HCID 100479 | — |
| 反応物 | 3,5-Diamino-2-methylbenzoic acid | HCID 135524 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | HCID 178497356 | HCID 178497356 | — |
反応手順
2.00 g (12.0 mmol) Methyl-3,4-diamino-benzoate were dissolved in 50 mL concentrated acetic acid. Then 2.09 mL (1.4 equiv.) methyl-2,2,2-trichloroacetimidate were added slowly and the resulting mixture was stirred at room temperature for 2 h. The mixture was diluted with 100 mL toluene and the solvent was removed under reduced pressure. The residue was taken up in dichloromethane and washed once with a saturated NaHCO3-solution and once with brine. The organic layer was dried over MgSO4 and the solvent was removed under reduced pressure to give pure methyl-2-trichloromethyl-1H-benzoimidazole-5-carboxylate as a light brown amorphous solid. Yield: 3.64 g MS (ES+): m/e=293, chloro pattern.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07741341B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-adba86b5f34648e9b32436231fe51488 |
| 出典メモ | uspto-grants-2010_06 |