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Hydrochloric Acid → 2-Methyl-N-[4-[(5(6H)-phenanthridinyl)carbonyl]phenyl]benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 5,6-Dihydrophenanthridine | HCID 219966 | — |
| 反応物 | 4-[(2-methylbenzoyl)amino]benzoyl Chloride | HCID 10707441 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 2-Methyl-N-[4-[(5(6H)-phenanthridinyl)carbonyl]phenyl]benzamide | HCID 15307971 | 18.9% |
反応手順
To a solution of 0.181 g (1.0 mmol) of 5,6-dihydrophenanthridine in 2 ml of warm pyridine is added 0.273 g (1.0 mmol) of 4-[(2-methylbenzoyl)amino]benzoyl chloride. The mixture is stirred overnight at room temperature, 1.2 ml of 2N HCl added. The solid which separates is filtered and washed with water. The solid is dissolved in dichloromethane and the solution washed with 2M sodium carbonate. The organic layer is concentrated and the residue chromatographed twice on silica gel with ethyl acetate-hexane as solvent to give 79 mg of crystals, m.p. 190°-194° C. Mass Spec-FAB 419 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05760031 |
| 出典データセット | uspto-grants-1998_06 |
| ORD ID | ord-68ef0fa7a5964731ad85617c54edad08 |
| 出典メモ | uspto-grants-1998_06 |