関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Piperidinecarboxylic acid | HCID 3773 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Dimethylacetamide | HCID 31374 | — |
| 反応物 | 3-Bromo-5-fluorobenzonitrile | HCID 2783330 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-(3-Bromo-5-cyanophenyl)piperidine-4-carboxylic acid | HCID 59588189 | — |
反応手順
A mixture of 3-bromo-5-fluorobenzonitrile (1.6 g, 7.8 mmol), piperidine-4-carboxylic acid (2.6 g, 12.0 mmol), triethylamine (4.0 mL, 28.5 mmol) and N,N-dimethylacetamide (1.5 mL) in a sealed tube was heated to 130° C. for 48 hr. The reaction mixture was diluted with EtOAc and water. The organic layer was separated, dried (MgSO4), and concentrated to give a crude reside which was purified by chromatography on silica gel (CH2Cl2/MeOH) to afford 1-(3-bromo-5-cyanophenyl)piperidine-4-carboxylic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09018205B2 |
|---|
| 出典データセット | uspto-grants-2015_04 |
|---|
| ORD ID | ord-d29d1020a44143528ce1a4ffac2d4325 |
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| 出典メモ | uspto-grants-2015_04 |
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