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Water → N-[4-(Pyrido[2,3-b][1,5]benzoxazepin-6(5H)-ylcarbonyl)-3-chlorophenyl][1,1'-biphenyl]-2-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 5,6-Dihydropyrido[2,3-b][1,5]benzoxazepine | HCID 15895929 | — |
| 反応物 | 4-[([1,1'-Biphenyl]-2-carbonyl)amino]-2-chlorobenzoyl chloride | HCID 22099600 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-[4-(Pyrido[2,3-b][1,5]benzoxazepin-6(5H)-ylcarbonyl)-3-chlorophenyl][1,1'-biphenyl]-2-carboxamide | HCID 22099925 | — |
反応手順
A mixture of 0.198 g of 5,6-dihydropyrido[2,3-b][1,5]benzoxazepine, 0.155 g of N,N-diisopropylethylamine and 0.444 g of 4-[([1,1-biphenyl]-2-carbonyl)amino]-2-chlorobenzoyl chloride in 12 ml of dichloromethane is stirred at room temperature for 2.5 hours. The mixture is poured into water and extracted with dichloromethane. The extract is washed with 2N Na2CO3, H2O, brine and dried (Na2 SO4). The solution is passed through a thin pad of hydrous magnesium silicate. The filter pad is washed with 50 ml of hexane-ethyl acetate (1:2) and the filtrate concentrated to dryness.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05849735 |
| 出典データセット | uspto-grants-1998_12 |
| ORD ID | ord-fe7620382d5a4248a662034564e8e059 |
| 出典メモ | uspto-grants-1998_12 |