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Methanol → Methyl 2-(4-fluorophenyl)acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 2-(4-Fluorophenyl)acetic acid | HCID 9837 | — |
| 溶媒 | Diethylether ethylacetate | HCID 21584169 | — |
| 生成物 | Methyl 2-(4-fluorophenyl)acetate | HCID 2733233 | — |
反応手順
A catalytic amount (0.5 mL) of concentrated sulfuric acid was added to a solution of 4-fluorophenylacetic acid (30.8 g, 0.20 mol) in 500 mL of methanol. The solution was stirred at reflux for 4 hours. The volatile materials were removed under reduced pressure to furnish a colorless oil which was dissolved in ether/ethyl acetate and washed with 2 N aqueous Na2CO3, brine, dried over MgSO4, and filtered. The filtrate was concentrated under reduced pressure to provide an oil which was dried overnight under high vacuum (yield: 33.6 g; 95%). 1H NMR (300 MHz, CDCl3) δ 3.59 (s, 2H), 3.65 (s, 3H), 7.01 (t, J=9 Hz, 2H), 7.20-7.28 (m, 2H). MS (DCI/NH3) m/z 186 (M+NH4)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06307047B1 |
| 出典データセット | uspto-grants-2001_10 |
| ORD ID | ord-6feb91dac7f34909bb374af84cd94bf1 |
| 出典メモ | uspto-grants-2001_10 |