化工社化工社 化学情報印刷レポート · 研究参考用
Trimethylsilyl cyanide → (8-ethoxy-4H-benzo[1,3]dioxin-6-yl)-[4-(5-methyl-[1,2,4]oxadiazol-3-yl)phenylamino]acetonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trimethylsilyl cyanide | HCID 82115 | — |
| 反応物 | Ytterbium triflate | HCID 2733225 | — |
| 反応物 | 4-(5-Methyl-1,2,4-oxadiazol-3-yl)aniline | HCID 18188176 | — |
| 反応物 | 8-ethyl-4H-benzo[1,3]dioxine-6-carbaldehyde | HCID 59517295 | — |
| 反応物 | 2-{3-[(4-carbamimidoylphenylamino)-(2-fluoro-4,5-dimethoxyphenyl)methyl]5-oxo-4,5-dihydro-[1,2,4]triazol-1-yl}benzoic Acid Trifluoroacetate | HCID 136337083 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (8-ethoxy-4H-benzo[1,3]dioxin-6-yl)-[4-(5-methyl-[1,2,4]oxadiazol-3-yl)phenylamino]acetonitrile | HCID 67096857 | — |
反応手順
To a solution of 230 mg of Yb(OTf)3 in 20 ml of dichloromethane there were added 650 mg of 4-(5-methyl-[1,2,4]oxadiazol-3-yl)phenylamine, 773 mg of 8-ethyl-4H-benzo[1,3]dioxine-6-carbaldehyde, 1g of MS3A and 0.8 ml of trimethylsilyl cyanide under a nitrogen atmosphere, and the mixture was stirred overnight at room temperature. The reaction mixture was filtered through celite, and the celite was washed with 100 ml of ethyl acetate. The organic layer was concentrated under reduced pressure to give (8-ethoxy-4H-benzo[1,3]dioxin-6-yl)-[4-(5-methyl-[1,2,4]oxadiazol-3-yl)phenylamino]acetonitrile (crude product).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07928228B2 |
| 出典データセット | uspto-grants-2011_04 |
| ORD ID | ord-d578f82abb86488794ad4376fa539596 |
| 出典メモ | uspto-grants-2011_04 |