化工社化工社 化学情報印刷レポート · 研究参考用
Water → 1-Ethyl-7-hydroxy-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Boron tribromide dichloromethane | HCID 22277759 | — |
| 反応物 | 1-Ethyl-7-methoxy-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione | HCID 68674307 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Dichloromethane methanol | HCID 21226129 | — |
| 生成物 | 1-Ethyl-7-hydroxy-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione | HCID 68673385 | 97.5% |
反応手順
1.0M-boron tribromide/dichloromethane solution (1.22 ml) was added to a dichloromethane solution (3 ml) of 1-ethyl-7-methoxy-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (169 mg) at 0° C. The mixture was stirred at room temperature overnight. Water and methanol were added to the reaction mixture, and extraction was performed using a dichloromethane/methanol mixture (dichloromethane:methanol=10:1). The organic layer was dried over anhydrous sodium sulfate, and condensed to dryness under reduced pressure to give the title compound (156.4 mg) as a white powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822453B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-9f866d02a8014aba85fdf27de5334129 |
| 出典メモ | uspto-grants-2014_09 |