関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Carbonic acid, monomethyl ester, magnesium salt (2:1) | HCID 167017 | — |
| 反応物 | 1-[5-(Tetradecyloxy)thiophen-2-yl]ethan-1-one | HCID 21427521 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 54275300 | HCID 54275300 | — |
反応手順
A mixture of magnesium methyl carbonate and dimethylformamide (300 g of a 2.0mM/g solution) is heated in a 120° C. oil bath with stirring under carbon dioxide flushing for 1/2 hour. To this mixture is added 33.8 g (0.100 mole) of 5-(tetradecyloxy)-2-thienyl methyl ketone, and the oil bath temperature is raised to 130° C. to 150° C. Dry nitrogen is flushed through the mixture for 5 hours. The mixture is allowed to cool at room temperature under carbon dioxide flushing after which it is poured slowly into 3 liters of concentrated HCl-ice (1:1) with vigorous stirring. When the evolution of gas is complete, the precipitate is collected and washed with cold water, then dried to give 5-tetradecyloxythen-2-oylacetic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04032647 |
|---|
| 出典データセット | uspto-grants-1977_06 |
|---|
| ORD ID | ord-895bb4a93b274cae807a6b1424eb3bc7 |
|---|
| 出典メモ | uspto-grants-1977_06 |
|---|