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1-(3-Hydroxy-4-methoxyphenyl)ethanone → 5-[(E)-N-[(2-fluorophenyl)methoxy]-C-methylcarbonimidoyl]-2-methoxyphenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-(3-Hydroxy-4-methoxyphenyl)ethanone | HCID 95693 | — |
| 反応物 | O-(2-Fluorobenzyl)hydroxylamine hydrochloride | HCID 21192890 | — |
| 溶媒 | Ethyl acetate hexane | HCID 21226206 | — |
| 生成物 | 5-[(E)-N-[(2-fluorophenyl)methoxy]-C-methylcarbonimidoyl]-2-methoxyphenol | HCID 25100408 | 91% |
反応手順
Acetophenone 12 (50 mg, 0.301 mmol) was condensed with O-(2-fluorobenzyl)hydroxylamine hydrochloride (32) (58 mg, 0.327 mmol) according to the general procedure II-B defined above. After being heated for 36 h the reaction mixture was cooled and the solvent removed under reduced pressure. The ensuing residue was dissolved in CH2Cl2 (15 mL) and the resulting solution washed with H2O (2×10 mL) then dried (MgSO4), filtered and concentrated under reduced pressure. The oil thus obtained was subjected to flash chromatography (1:19 v/v ethyl acetate/hexane) to afford the title compound CP30280 (79 mg, 91%) as a pale-yellow oil, Rf 0.5 in 1:1 v/v ethyl acetate/hexane.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08536157B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-a1cb47cc8f73450e8f575565cb87c1e6 |
| 出典メモ | uspto-grants-2013_09 |