関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl bromopyruvate | HCID 66144 | — |
| 反応物 | tert-Butyl 4-carbamothioylpiperidine-1-carboxylate | HCID 2735648 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-Piperidine-4-yl-thiazole-4-carboxylic acid ethyl ester | HCID 57935959 | — |
反応手順
A mixture of 10 g (41 mmol) 4-thiocarbamoyl-piperidine-1-carboxylic acid tert-butyl ester (commercially available) and 7.98 g (41 mmol) ethyl bromopyruvate (commercially available) in 120 ml ethanol was stirred at 70° C. for 90 min. The mixture was evaporated to dryness, Na2CO3 aq. was added and the residue was extracted with ethyl acetate. The organic phases were washed with NaCl aq., dried with MgSO4 and evaporated to dryness. The residue was purified on silica eluting with DCM/MeOH/25% NH3 in water 100/20/1 to yield after evaporation of the product fractions 7.28 g (74%) of the title compound as light brown solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07786143B2 |
|---|
| 出典データセット | uspto-grants-2010_08 |
|---|
| ORD ID | ord-0d3c725b12274cf9a1c6d1826071b2fb |
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| 出典メモ | uspto-grants-2010_08 |
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