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Ethyl 3-methyl-5-[4-(trifluoromethyl)phenyl]thiophene-2-carboxylate → {2-Methyl-5-[4-(trifluoromethyl)phenyl]thien-3-yl}methanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl 3-methyl-5-[4-(trifluoromethyl)phenyl]thiophene-2-carboxylate | HCID 15946279 | — |
| 反応物 | Sodium Bisulfite | HCID 23665763 | — |
| 反応物 | Sodium Bromate | HCID 23668195 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Cyclohexane | HCID 8078 | — |
| 生成物 | {2-Methyl-5-[4-(trifluoromethyl)phenyl]thien-3-yl}methanol | HCID 21986536 | — |
反応手順
Ethyl 3-methyl-5-[4-(trifluoromethyl)phenyl]thiophene-2-carboxylate (intermediate 35, 0.100 g) and sodium bromate (0.144 g) were suspended in a mixture of cyclohexane and water (1:1 v/v, 4 ml). To this was added a solution sodium bisulfite (0.99 g) in water (1 ml). The mixture was stirred for 2 hours, quenched with 1M sodium thiosulfate solution, then extracted with ethyl acetate. The organic layer was taken and washed with water, sodium thiosulfate and dried with brine and over MgSO4 and concentrated to give the title compound as a white crystalline solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07091237B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-01fd9acbd4244adfb8428d8144a29522 |
| 出典メモ | uspto-grants-2006_08 |