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2-Methylbenzoyl chloride → N-[4-(5H-Pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)ylcarbonyl)-2-methylphenyl]-2-methylbenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Methylbenzoyl chloride | HCID 70276 | — |
| 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-methylbenzamide | HCID 21837166 | 65.9% |
反応手順
A solution of 0.83 g of 10,11-dihydro-10-(4-amino-3-methylbenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 0.5 g of N,N-diisopropylethylamine and 0.6 g of 2-methylbenzoyl chloride in 50 ml of methylene chloride is stirred at room temperature for 18 hours. The reaction mixture is washed with water, the organic layer dried with Na2SO4 and passed through a pad of hydrous magnesium silicate. Hexane is added at the boil to give 0.75 g of a solid which is crystallized from methylene chloride-hexane to give 0.61 g of the desired product, m.p. 125°-130° 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-a0865d39ece04d7ca18701901cb148a2 |
| 出典メモ | uspto-grants-1998_03 |