関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Methyl 2-chloropropanoate, (R)- | HCID 149593 | — |
| 反応物 | 4-Fluoro-3-(3-hydroxypropyl)phenol | HCID 68536325 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | methyl(2S)-2-[4-fluoro-3-(3-hydroxypropyl)phenoxy]propanoate | HCID 68533499 | 66.8% |
反応手順
To a mixture of 4-fluoro-3-(3-hydroxypropyl)phenol (1.5 g), methyl (2R)-2-chloropropanoate (1.30 g) in DMSO (7.5 mL) was added Cs2CO3 (3.45 g) at ambient temperature. The mixture was stirred at 60° C. for 3 hours. After cooling to ambient temperature, the reaction mixture was diluted with EtOAc (50 mL) and washed successively with water (30 mL) two times and brine (30 mL). The organic layer was dried over anhydrous MgSO4, filtered and evaporated in vacuo to give crude oil. The crude oil was purified by silica gel column chromatography (n-hexane:EtOAc=4:1-2:1) to give methyl(2S)-2-[4-fluoro-3-(3-hydroxypropyl)phenoxy]propanoate (1.51 g) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08273745B2 |
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| 出典データセット | uspto-grants-2012_09 |
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| ORD ID | ord-6c2c0f1bedca4ae4af36eb8e4e219608 |
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| 出典メモ | uspto-grants-2012_09 |
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