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Sulfuric Acid → Methyl 4-phenylpiperidine-4-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 4-Piperidinecarboxylic acid, 4-phenyl-, 4-methylbenzenesulfonate (1:1) | HCID 2723657 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methyl 4-phenylpiperidine-4-carboxylate | HCID 545827 | — |
反応手順
To a stirred solution of H2SO4 (16 mL) in MeOH (400 mL), 4-phenyl-4-piperidinecarboxylic acid 4-methyl benzenesulfonate (37.7 g, 0.1 mole) was added and the mixture was stirred and refluxed for 8 hours. Excess methanol was evaporated at reduced pressure and the residue was poured into a mixture of ice and 6 N NaOH. The pH was adjusted to 10-11 by adding more 6 N NaOH and extracted with CH2Cl2 (3×150 mL). The combined CH2Cl2 extracts were dried (MgSO4) and the solvent evaporated to leave the desired product as a viscous oil. The product (20.2 g, 92%) was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06218390B1 |
| 出典データセット | uspto-grants-2001_04 |
| ORD ID | ord-b55eaf45509740169295d7897492606a |
| 出典メモ | uspto-grants-2001_04 |