関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloromethyl Methyl Ether | HCID 7864 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Fluoro-3-hydroxybenzoic acid | HCID 593635 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-Fluoro-3-(methoxymethoxy)benzyl alcohol | HCID 23074311 | 94% |
反応手順
Triethylamine (1.07 mL) and methoxymethyl chloride (2.24 mL) were added to tetrahydrofuran (10 mL) solution of 4-fluoro-3-hydroxybenzoic acid (1.0 g), and stirred at 0° C. for 2 hours. Ethyl acetate was added to the reaction liquid which then was washed with water and saturated brine, dried over anhydrous magnesium sulfate, the solvent therein was concentrated under reduced pressure and the residue was dissolved in tetrahydrofuran (20 mL). Lithiumaluminium hydride (360 mg) was added, stirred at 0° C. for an hour, ethyl acetate was added and the insoluble matter was removed, followed by washing with saturated brine and drying over anhydrous magnesium sulfate. Concentrating the solvent under reduced pressure, the title compound (1.14 g, 94%) was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07732456B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-b32e232e6caf496cb7414acd838cedd1 |
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| 出典メモ | uspto-grants-2010_06 |
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