関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | N-(1-(2,2-dimethoxyethyl)-1H-pyrazol-4-yl)-5-(m-tolyl)oxazole-4-carboxamide | HCID 86704230 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-(1-(2-oxoethyl)-1H-pyrazol-4-yl)-5-(m-tolyl)oxazole-4-carboxamide | HCID 86704232 | — |
反応手順
To N-(1-(2,2-dimethoxyethyl)-1H-pyrazol-4-yl)-5-(m-tolyl)oxazole-4-carboxamide (800 mg, 2.25 mmol) in THF (11.5 mL), 2 N aq. HCl-solution (10.3 mL, 20.60 mmol) was added dropwise and the resulting solution was refluxed (80° C.) for 1.5 h. The reaction mixture was allowed to reach rt, then neutralized with sat. aq. NaHCO3-solution and the org. solvent was removed under reduced pressure. The remaining aq. layer was extracted with EtOAc (2×) and the combined org. layer were washed with brine, dried (MgSO4), filtered and concentrated to obtain the title compound as a yellow solid which was used immediately in the next step. LC-MS conditions C: tR=0.72 min, [M+H2O+H]+=329.09.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09303023B2 |
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| 出典データセット | uspto-grants-2016_04 |
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| ORD ID | ord-c22a4353ed574bde9b528ce25ba8b965 |
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| 出典メモ | uspto-grants-2016_04 |
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