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2-Chlorotoluene → O-(6,6-difluoro-5-methyl-5-hexenyl) benzo[b]thiophene-2-thiocarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Chlorotoluene | HCID 7238 | — |
| 反応物 | Diisopropyl Ether | HCID 7914 | — |
| 反応物 | Lawesson's reagent | HCID 87949 | — |
| 反応物 | 6,6-Difluoro-5-methyl-5-hexenyl benzo[b]thiophene-2-carboxylate | HCID 69181690 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | O-(6,6-difluoro-5-methyl-5-hexenyl) benzo[b]thiophene-2-thiocarboxylate | HCID 86760554 | 81.4% |
反応手順
To 5 ml of 2-chlorotoluene was dissolved 0.20 g (0.64 mmol) of 6,6-difluoro-5-methyl-5-hexenyl benzo[b]thiophene-2-carboxylate, followed by the addition of 0.26 g (0.64 mmol) of Lawesson's reagent and stirring by heating under refluxing for 4 hours. To the reaction liquid were added 2 ml of isopropyl ether and 10 ml of hexane and precipitated solid was filtered off. The filtrate was concentrated under reduced pressure and the residue was purified with silica gel column chromatography (diisopropyl ether:hexane=1:30) to obtain 0.17 g (yield: 81%) of O-(6,6-difluoro-5-methyl-5-hexenyl) benzo[b]thiophene-2-thiocarboxylate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07273878B2 |
| 出典データセット | uspto-grants-2007_09 |
| ORD ID | ord-54f3d4c86d6c4f1483707799d247ea36 |
| 出典メモ | uspto-grants-2007_09 |