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Methanol → Methyl (3-(trifluoromethyl)phenyl)acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 3-(Trifluoromethyl)benzeneacetic acid | HCID 67695 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Methyl (3-(trifluoromethyl)phenyl)acetate | HCID 2734603 | 89% |
反応手順
Into a solution of 3-trifluoromethylphenylacetic acid (20.0 g. 98 mmol) in MeOH (100 mL), cooled in an ice-water bath, was bubbled HCl (g) for 15 min. The mixture was allowed to warm to room temperature and was then concentrated in vacuo to furnish a clear, yellow-green liquid which was diluted with EtOAc (0.25L) and washed with saturated aqueous NaHCO3 (2×0.25L), brine (0.25L), and dried (Na2SO4). Concentration in vacuo provided the crude ester which was purified by chromatography on a column of silica gel(230-400 mesh, 600 g, 70 mm o.d., ethyl acetate-hexanes 10:90, 400 mL fractions) using the flash technique. Fractions 6-9 provided 19.08 g (89%) of methyl-3-trifluoromethylphenylacetate as a clear colorless liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05245046 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-1e607e457e3c44ccb98525fa715b1116 |
| 出典メモ | uspto-grants-1993_09 |