化工社化工社 化学情報印刷レポート · 研究参考用
N-vinyl-2-pyrrolidone → 3-Chloro-8-methoxy-7-[1-(2-oxopyrrolidin-1-yl)vinyl]-5,10-dihydro-11h-dibenzo[b,e][1,4]diazepin-11-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-vinyl-2-pyrrolidone | HCID 6917 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-chloro-8-methoxy-11-oxo-10,11-dihydro-5H-dibenzo[b,e][1,4]diazepin-7-yl trifluoromethanesulfonate | HCID 87738200 | — |
| 触媒 | HCID 178418807 | HCID 178418807 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-Chloro-8-methoxy-7-[1-(2-oxopyrrolidin-1-yl)vinyl]-5,10-dihydro-11h-dibenzo[b,e][1,4]diazepin-11-one | HCID 69217774 | — |
反応手順
A mixture of Example 516A, 1-vinyl-2-pyrrolidinone, Pd(dppf)Cl2-CH2Cl2, and triethylamine in DMF was heated at 110° C. overnight, cooled to room temperature, diluted with ethyl acetate, washed with water and brine, dried (MgSO4), filtered and concentrated. The concentrate was purified by column chromatography on silica gel using a solvent gradient that increased from 1 to 4% methanol in dichloromethane to give the title compound. MS (ESI) m/e 384 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07456169B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-ef4269893cc14acf92ab779d66eb474b |
| 出典メモ | uspto-grants-2008_11 |