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2,4-Dichlorobenzoyl chloride → N-[4-(5H-Pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)ylcarbonyl]-2-methylphenyl]-2,4-dichlorobenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,4-Dichlorobenzoyl chloride | HCID 66645 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 10,11-Dihydro-10-(4-amino-3-methylbenzoyl)-5H-Pyrrolo[2,1-c][1,4]benzodiazepine | HCID 10686975 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-[4-(5H-Pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)ylcarbonyl]-2-methylphenyl]-2,4-dichlorobenzamide | HCID 10743659 | 84.1% |
反応手順
A mixture of 0.40 g of 10,11-dihydro-10-(3-methyl-4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 0.40 g of 2,4-dichlorobenzoyl chloride and 0.75 g of diisopropylethylamine in 50 ml of dichloromethane is stirred at room temperature for 16 hours. The mixture is washed with water, dried (MgSO4) and the solution passed through a thin pad of hydrous magnesium silicate. The filtrate is concentrated and hexane added to give crystals. Recrystallization from dichloromethane-hexane gives 0.52 g of crystals, m.p. 213°-215° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05733905 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-f0f4f088cd0d48ca83f5762cc569ed4f |
| 出典メモ | uspto-grants-1998_03 |