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Water → Acetic acid, 2-[4-[[4,4''-bis(trifluoromethyl)[1,1':3',1''-terphenyl]-5'-yl]methoxy]-2-methylphenoxy]-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 反応物 | [4-(3,5-Bis(4-trifluoromethylphenyl)-benzyloxy)-2-methyl-phenoxy]-acetic acid methyl ester | HCID 59007659 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Acetic acid, 2-[4-[[4,4''-bis(trifluoromethyl)[1,1':3',1''-terphenyl]-5'-yl]methoxy]-2-methylphenoxy]- | HCID 11649783 | — |
反応手順
The crude [4-(3,5-bis(4-trifluoromethylphenyl)-benzyloxy)-2-methyl-phenoxy]-acetic acid methyl ester from Step A above is dissolved in dioxane (2 mL). Solid lithium hydroxide monohydrate (18 mg, 0.44 mmol, excess) is added, followed by water (0.2 mL). After 1 hour, the mixture is concentrated to dryness. Purification by reversed-phase HPLC yields [4-(3,5-bis(4-trifluoromethylphenyl)-benzyloxy)-2-methyl-phenoxy]-acetic acid A1 as a solid. 1H-NMR (400 MHz, CDCl3) δ=7.67 (m, 9H), 7.61 (s, 2H), 6.82 (d, J=2.8 Hz, 1H), 6.72 (dd, J=9.0, 2.8 Hz, 1H), 6.64 (d, J=9.2 Hz, 1H), 5.08 (s, 2H), 4.58 (s, 2H), 2.22 (s, 3H). 19F-NMR (376 MHz, CDCl3) δ=−62.4. No MS could be obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07745445B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-0cc6a5ba7350470187529b974bbc1faa |
| 出典メモ | uspto-grants-2010_06 |