化工社化工社 化学情報印刷レポート · 研究参考用
Diisopropylethylamine → trans-N-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)-4-phenylbenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 4-Phenylbenzoyl chloride | HCID 84151 | — |
| 反応物 | trans-7-Chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine maleate | HCID 86599859 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | trans-N-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)-4-phenylbenzamide | HCID 86599861 | 47.8% |
反応手順
DIPEA (18.6 μL, 0.14 mmol) and 4-phenylbenzoyl chloride (15.2 mg, 0.07 mmol) were added to a solution of trans-7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine maleate (9.6 mg, 0.02 mmol) in 1 mL of CH2Cl2. The resulting mixture was stirred for 18 h at room temperature. The organic layer was washed with 5% aqueous sodium bicarbonate and H2O, dried (Na2SO4) and evaporated. Additional chromatography on silica (elution with toluene/ethyl acetate 9:1→toluene/ethyl acetate 1:1) gave trans-N-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)-4-phenylbenzamide (4.6 mg, 44%). Data: (m/z)=350 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07737136B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-36620f0501694e209f7346bd72b71148 |
| 出典メモ | uspto-grants-2010_06 |