関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloroacetic Acid | HCID 300 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 3,4-Dichlorobenzyl chloride | HCID 7609 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Thiourea | HCID 2723790 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178526174 | HCID 178526174 | 89.3% |
反応手順
A mixture of 19.5 g (0.1 mol) of 3,4-dichlorobenzylchloride and 7.6 g (0.1 mol) of thiourea in 50 ml of water are heated under reflux for 30 minutes with stirring, and then a solution of 16 g (0.4 mol) of NaOH in 25 ml of water is run in at 60°-70° C.; the mixture is heated under reflux for 15 minutes, a solution of 15 g (0.15 mol) of chloroacetic acid, 7 g of sodium carbonate and 50 ml of water is run in at 60°-70° C., and the mixture is maintained under reflux for 1 hour. The mixture is acidified cold with concentrated HCl, extracted with ether, and the extract is washed with water, dried and evaporated. The residue is taken up in petroleum ether and filtered off. 21 g of the stated product are obtained (yield: 83%) melting point: 63°-64° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04225617 |
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| 出典データセット | uspto-grants-1980_09 |
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| ORD ID | ord-82f0ccebe0c344529afcf12476748e39 |
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| 出典メモ | uspto-grants-1980_09 |
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