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Acetone → Ethyl 4-nitrobenzylthioacetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ethyl Thioglycolate | HCID 12185 | — |
| 反応物 | 4-Nitrobenzyl bromide | HCID 66011 | — |
| 触媒 | Potassium Iodide | HCID 4875 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Ethyl 4-nitrobenzylthioacetate | HCID 54092468 | 95% |
反応手順
43.2 g (0.2 mol) of p-nitrobenzyl bromide, 200 ml of acetone, 0.2 g of potassium iodide, 24 ml of ethyl thioglycollate (that is to say a slight excess) and 27.6 g (0.2 mol) of potassium carbonate are introduced successively into a 1 liter three-necked flask. The mixture is heated under reflux for about 4 hours until the complete disappearance of the bromo derivative; the acetone is evaporated, the oil obtained is taken up in ether and in water, the ether phase is washed with a dilute NaOH solution, so as to eliminate the excess thiol, and then with a dilute HCl solution, and is dried over Na2SO4, and the solvent is evaporated. 49 g (yield: 95%) of the stated product are obtained, which is in the form of an orange-coloured oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04325964 |
| 出典データセット | uspto-grants-1982_04 |
| ORD ID | ord-81193c2ac0604414b08ba8be037c0959 |
| 出典メモ | uspto-grants-1982_04 |