関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Thioglycolic Acid | HCID 1133 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 2-Bromo-1,4-dichlorobenzene | HCID 15033 | — |
| 反応物 | 2,3-Dichlorobenzenethiol | HCID 140202 | — |
| 反応物 | Dichlorophenylthioglycolate | HCID 86746840 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 2-(2,5-Dichlorophenyl)-2-mercaptoacetic acid | HCID 22492329 | 60.5% |
反応手順
To a 500 ml flask equipped with a thermometer, a condenser and a stirrer were added 45.2 g (0.2 mol) of 1-bromo-2,5-dichlorobenzene, 23.7 g (0.4 mol) of 95% potassium hydroxide, 18.4 g (0.2 mol) of thioglycolic acid and 320 g of N-methyl-2-pyrrolidone, followed by stirring at 140° to 150° C. for 2 hours. Assay of the reaction solution by high performance liquid chromatography identified the solution as a mixture of dichlorophenylthioglycolate and dichlorothiophenol salt. Then, after distilling off the solvent, 300 g of water and 50 g of toluene were added for layer separation. To the water layer was added 45 g of concentrated hydrochloric acid, and the mixture was cooled to room temperature. The resulting crystal was filtered and dried to yield 28.7 g of 2,5-dichlorophenylthioglycolic acid. Its melting point was 129° to 131° C., and the yield was 60.5%. The results are given in Table 2.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05210291 |
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| 出典データセット | uspto-grants-1993_05 |
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| ORD ID | ord-a8496bce6d5e4e34bf39273275a81065 |
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| 出典メモ | uspto-grants-1993_05 |
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