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2-Bromo-1-(4-fluorophenyl)ethan-1-one → Tert-butyl 4-[2-(4-fluorophenyl)-2-oxoethyl]piperazine-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Bromo-1-(4-fluorophenyl)ethan-1-one | HCID 96749 | — |
| 反応物 | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Tert-butyl 4-[2-(4-fluorophenyl)-2-oxoethyl]piperazine-1-carboxylate | HCID 46901916 | 40.5% |
反応手順
tert-Butyl piperazine-1-carboxylate (5.00 g, 26.8 mmol) and 2-bromo-1-(4-fluorophenyl)ethanone (6.99 g, 32.2 mmol) were dissolved in DMF (5 mL) and stirred for 10 min at room temperature. The crude material was purified by column chromatography eluting with a mixture of DCM and MeOH to afford the title compound (3.50 g) as an oil. 1H NMR (Acetonitrile-d3, 400 MHz) δ 1.42 (s, 9H) 2.47 (t, J=5.0 Hz, 4H), 3.36 (t, J=5.0 Hz, 4H), 3.77 (s, 2H), 7.20 (t, J=8.8, 2H), 8.07 (td, J=2.0, 8.8 Hz, 2H). Exact mass calculated for C17H23FN2O3: 322.2. Found: LCMS m/z=323.4 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09434692B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-70316a9a9e62437d99687124d694f523 |
| 出典メモ | uspto-grants-2016_09 |