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Diethyl Ether → Ethyl 4-nitrobenzylthioacetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ethyl Thioglycolate | HCID 12185 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | 4-Nitrobenzyl bromide | HCID 66011 | — |
| 触媒 | Potassium Iodide | HCID 4875 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Ethyl 4-nitrobenzylthioacetate | HCID 54092468 | 95% |
反応手順
43.2 g (0.2 mol) of p-nitrobenzylbromide, 200 ml of acetone, 0.2 g of potassium iodide, 24 ml of ethyl thioglycolate (namely a slight excess) and 27.6 g (0.2 mol) of potassium carbonate are successively introduced into a 1 liter 3-necked flask. The mixture is heated under reflux for about 4 hours until the bromine derivative completely disappears; the acetone is evaporated, the oil obtained is taken up in ether and in water, the ether phase is washed with a dilute solution of NaOH to remove the excess thiol, and then with a dilute solution of HCl, the solution is dried over Na2SO4 and the solvent is evaporated off. 49 g (yield: 95%) of the stated product, which is in the form of an orange coloured oil, are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04151300 |
| 出典データセット | uspto-grants-1979_04 |
| ORD ID | ord-3b644a4d9d3b4bcca874389de95ab514 |
| 出典メモ | uspto-grants-1979_04 |