関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dopac | HCID 547 | — |
| 反応物 | Diethyl Sulfate | HCID 6163 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Potassium bisulfate | HCID 516920 | — |
| 反応物 | Barium hydroxide, octahydrate | HCID 17749109 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3,4-Diethoxyphenylacetic acid | HCID 579813 | — |
反応手順
0.8 g of 3,4-dihydroxy-phenylacetic acid and 6.9 g of barium hydroxide octahydrate are dissolved in 50 ml of water and at ambient temperature 2.9 ml of diethylsulphate are added dropwise. The solution is stirred for 2 hours at ambient temperature and for 2 hours at 40° C. After this time the solution is acidified with saturated potassium hydrogen sulphate solution, mixed with ethyl acetate and the suspension is filtered through Celite. The phases are separated and the ethyl acetate phase is dried over sodium sulphate and concentrated by evaporation. The residue obtained is purified through a silica gel column with toluene/ethyl acetate/ethanol (4:2:1) as eluant.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06794395B1 |
|---|
| 出典データセット | uspto-grants-2004_09 |
|---|
| ORD ID | ord-4b67fc642c024da69356a00d8d3e23ff |
|---|
| 出典メモ | uspto-grants-2004_09 |
|---|