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Ethyl Acetate → 4-(Aminosulfonyl)-N-{(cis)-2-[({[(3-chlorophenyl)sulfonyl]amino)acetyl)amino]cyclohexyl}benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 3-Chlorobenzenesulphonyl chloride | HCID 17909 | — |
| 反応物 | N-(cis)-{2-[(aminoacetyl)amino]cyclohexyl}-4-(aminosulfonyl)benzamide hydrogen bromide | HCID 68830145 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(Aminosulfonyl)-N-{(cis)-2-[({[(3-chlorophenyl)sulfonyl]amino)acetyl)amino]cyclohexyl}benzamide | HCID 68828068 | 29.4% |
反応手順
N-(cis)-{2-[(aminoacetyl)amino]cyclohexyl}-4-(aminosulfonyl)benzamide hydrogen bromide, (61b), (70 mg) was dissolved in DMF (2.5 mL) prior to the addition of 3-chlorobenzenesulfonyl chloride (51 mg). After stirring overnight, EtOAc was added and the solution was washed with 1N HCl. The EtOAc was dried, filtered, and concentrated. Reverse phase HPLC purification (gradient elution, water/acetonitrile/TFA) of the resulting residue provided the title benzamide (25 mg). MS found: (M+H)+=530.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06706712B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-dcc707d7869046489fcea5627c8f95db |
| 出典メモ | uspto-grants-2004_03 |