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Triethylamine → N-[4-[(5,11-dihydro-10H-dibenz[b,e](1,4]diazepin-5-yl)carbonyl]phenyl]-2-methylbenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 10,11-Dihydro-5h-dibenzo[b,e][1,4]diazepine | HCID 36046 | — |
| 反応物 | 4-[(2-methylbenzoyl)amino]benzoyl Chloride | HCID 10707441 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-[4-[(5,11-dihydro-10H-dibenz[b,e](1,4]diazepin-5-yl)carbonyl]phenyl]-2-methylbenzamide | HCID 67624893 | — |
反応手順
A mixture of 1.0 g of 5,11-dihydro-10H-dibenz [b,e] [1,4]diazepine 1.9 g of 4-[(2-methylbenzoyl) amino]benzoyl chloride, 4 ml of triethylamine and 0.2 g of 4-(dimethylamino)pyridine in 60 ml of methylene chloride is stirred at room temperature for 18 hours. The reaction mixture is poured into ice water and the separated organic layer washed with 50 ml each of water, 2N HCl, water, saturated NaHCO3 and water. The organic layer is dried (Na2SO4) and the solvent removed to give a residue. The residue is chromatographed on a silica gel column using 1:4 ethyl acetate-hexane to give 1.8 g of the desired product as a solid, m.p. 68°-71° C.
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-18fe0cefdc9e437f9590799a74919879 |
| 出典メモ | uspto-grants-1998_06 |