関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| 反応物 | Methyl 3,5-dihydroxyphenylacetate | HCID 579787 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 57666065 | HCID 57666065 | — |
反応手順
Trifluoromethanesulphonic anhydride (7.05 g, 25.0 mmol) was added dropwise to a solution of 3,5-dihydroxyphenyl acetic acid methyl ester (1.80 g, 10.0 mmol) and pyridine (4.9 mL, 60.0 mmol) in DCM (20 mL) at 0° C. The temperature was maintained at 0° C. for 15 mins before warming to room temperature and the mixture stirred for 18 hrs. The reaction was diluted with DCM washed with H2O, Na2CO3, dil. HCl, brine, dried (MgSO4) and evaporated under reduced pressure to give a yellow oil. The residue was purified by flash column chromatography (EtOAc:petroleum ether), yield 4.0 g (89%), 1H NMR (CDCl3) δ 7.31 (d, 2H), 7.17 (t, 1H), 3.74 (s, 3H), 7.73 (s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08106236B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-10cdcfd1f2534856853208137ba24cd5 |
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| 出典メモ | uspto-grants-2012_01 |
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