関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 反応物 | 1-Bromo-2-(methoxymethyl)benzene | HCID 12927162 | — |
| 反応物 | Oxalic acid monomethyl ester chloride | HCID 86640482 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Methyl 2-methoxymethylphenylglyoxylate | HCID 19937173 | 57.7% |
反応手順
500 ml of an ethereal 1 M zinc chloride solution was dripped into a Grignard solution prepared from 12.0 g (0.46 mol) of magnesium shavings and 99.5 g (0.5 mol) of 1-bromo-2-methoxymethylbenzene in 500 ml of THF. The mixture was then refluxed for 1 hours, and a solution of 61.2 g (0.5 mol) of oxalic acid methyl ester chloride in 100 ml of THF was dripped in at an internal temperature of (-10)°C. After the mixture had been heated to about 20° C. it was stirred for a further 20 hours and then hydrolyzed with saturated ammonium chloride solution. After extraction with ether the combined ether phases were washed with water, dried and evaporated down. There was obtained 60 g of product (57.7%) as a mobile liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05298527 |
|---|
| 出典データセット | uspto-grants-1994_03 |
|---|
| ORD ID | ord-2dc1ba16547544328f2c8be48f369ed1 |
|---|
| 出典メモ | uspto-grants-1994_03 |
|---|
