関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Ethyl 4-bromobutyrate | HCID 76300 | — |
| 反応物 | 2,4-Dihydroxybenzamide | HCID 76601 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(4-Carbamoyl-3-hydroxy-phenoxy)-butyric Acid Ethyl Ester | HCID 12072783 | — |
反応手順
To 2,4-dihydroxybenzamide (16.5 g, 108.3 mmol) in DMF (100 mL) was added Cs2CO3 (39.0 g, 119.1 mmol) followed by ethyl 4-bromobutyrate (17.0 mL, 119.1 mmol). The mixture was heated to 70° C. for 2 h, cooled, diluted with water and extracted with EtOAc. The combined extracts were washed with water, dried over magnesium sulfate, concentrated, and chomatographed over silica gel (60% EtOAc/hexane) to a white solid (4.2 g, 15%). MS [M+H]− 267.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06482852B2 |
|---|
| 出典データセット | uspto-grants-2002_11 |
|---|
| ORD ID | ord-e023bd4d004e4caab7c8c9cb3c4e9bee |
|---|
| 出典メモ | uspto-grants-2002_11 |
|---|
