関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Acetate | HCID 517165 | — |
| 反応物 | 3-[2-(4-Bromo-phenyl)-2-oxo-ethylcarbamoyl]-pyrrolidine-1-carboxylic acid tert-butyl ester | HCID 59611512 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | tert-Butyl 3-(5-(4-bromophenyl)-1H-imidazol-2-yl)pyrrolidine-1-carboxylate | HCID 59611262 | 56.3% |
反応手順
A mixture of 3-[2-(4-bromo-phenyl)-2-oxo-ethylcarbarnoyl]-pyrrolidine-1-carboxylic acid tert-butyl ester (1.5 g, 3.6 mmol) and ammonium acetate (1.4 g, 18.2 mmol) in xylene (15 mL) was heated in a sealed tube at 140° C. for 2 hours. The volatile component was removed in vacuo, and the residue was dissolved in ethyl acetate (150 mL), washed with NaHCO3 solution, water and brine, dried over Na2SO4, filtered and concentrated in vacuo. The obtained residue was purified by flash chromatography to provide the desired product as a white solid (795 mg, 56%). m/z 391.8, 393.8 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08841278B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-f9cdcd56d7d24f078f264fdfc8aad99b |
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| 出典メモ | uspto-grants-2014_09 |
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