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Methyl Ethyl Ketone → 2,3-Difluoro-4'-(6-hydroxyhexyl)oxybiphenyl
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl Ethyl Ketone | HCID 6569 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 6-Bromo-1-hexanol | HCID 77970 | — |
| 反応物 | 4-(2,3-Difluorophenyl)phenol | HCID 18920834 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2,3-Difluoro-4'-(6-hydroxyhexyl)oxybiphenyl | HCID 18920840 | 63.8% |
反応手順
First, 5 g of 6-bromo-1-hexanol, 5.7 g of 2,3difluoro-4'-hydroxybiphenyl, 7.6 g of potassium carbonate, and 70 ml of methyl ethyl ketone were placed in a 100 ml flask. Then, the mixture was stirred under reflux for 20 hours. The reaction mixture was poured into water, and an organic layer was extracted with toluene. The toluene layer was washed with water and dried over anhydrous sodium sulfate. Thereafter, the solvent was distilled away. The residue was recrystallized from acetone to obtain 5.4 g of 2,3-difluoro-4'-(6-hydroxyhexyl)oxybiphenyl (Y: 63.5%). The compound thus obtained had a purity of 99.9% by GC.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05750213 |
| 出典データセット | uspto-grants-1998_05 |
| ORD ID | ord-be28440a12e4484a887f9ddf837cce26 |
| 出典メモ | uspto-grants-1998_05 |