化工社化工社 化学情報印刷レポート · 研究参考用
Water → N-[4-[(5,11-Dihydro-10H-dibenz[b,e][1,4]diazepin-10-yl)carbonyl]-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 | 10,11-Dihydro-5h-dibenzo[b,e][1,4]diazepine | HCID 36046 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 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-[(5,11-Dihydro-10H-dibenz[b,e][1,4]diazepin-10-yl)carbonyl]-3-chlorophenyl][1,1'-biphenyl]-2-carboxamide | HCID 22099587 | 58.6% |
反応手順
A mixture of 0.196 g of 5,11-dihydro-10H-dibenzo[b,e][1,4]diazepine, 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 overnight. The mixture is poured into water and extracted with dichloromethane. The extract is washed with 2N K2CO3, H2O, brine and dried (Na2 SO4). The solution is filtered through a thin pad of hydrous magnesium silicate. The filtrate is concentrated to dryness and the residue triturated with ether and the solvent removed. The residue is triturated with dichloromethane to give 0.31 g of solid, m.p. 158° C.-184° C. Anal. Found for C33H24ClN3O2 1/2 H2O; C,73.7; H, 4.6; N,7.5; Cl,6.9.
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-5bbc1f50d4854d4591f113cea24b666b |
| 出典メモ | uspto-grants-1998_12 |