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Methylparaben → Methyl 4-[2-(N-BOC-4-Piperidinyl)ethyloxy]benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylparaben | HCID 7456 | — |
| 反応物 | Tert-butyl 4-(2-iodoethyl)piperidine-1-carboxylate | HCID 9974426 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Methyl 4-[2-(N-BOC-4-Piperidinyl)ethyloxy]benzoate | HCID 10832539 | — |
反応手順
A solution of methyl 4-hydroxybenzoate (Aldrich) (0.4 g, 2.6 mmoles) 9-1 in DMF (10 ml) was treated with 2-(N-Boc-4-piperidinyl)ethyl iodide 1-4 (0.6 g, 1.77 mmoles) and CS2CO3 (1.15 g, 3.5 mmoles) with stirring at room temperature for 48 hours. The reaction mixture was diluted with EtOAc, washed with H2O, saturated NaHCO3, 10% KHSO4, brine dried (MgSO4) and concentrated. The residue was purified by flash chromatography on silica gel eluting with 20% EtOAc/hexanes to give pure 9-2. Rf 0.3.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05648368 |
| 出典データセット | uspto-grants-1997_07 |
| ORD ID | ord-b79d2a287dc44b13910f9db9d2875f8f |
| 出典メモ | uspto-grants-1997_07 |