関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Methylimidazole | HCID 1390 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | (3S)-2-[(2R)-3-cyclopentyl-2-({formyl[(phenylmethyl)oxy]amino}methyl)propanoyl]-1-{[(phenylmethyl)oxy]carbonyl}-3-pyrazolidinecarboxylic acid | HCID 86706346 | — |
| 反応物 | HCID 178507601 | HCID 178507601 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 178523396 | HCID 178523396 | 51.1% |
反応手順
To a solution of (3S)-2-[(2R)-3-cyclopentyl-2-({formyl[(phenylmethyl)oxy]amino}methyl)propanoyl]-1-{[(phenylmethyl)oxy]carbonyl}-3-pyrazolidine carboxylic acid (176 mg, 0.327 mmol) in DMF (2 ml) was added 1-methylimidazole (52 μl, 0.655 mmol) and cooled to 0° C. Mesyl chloride (27 μL, 0.344 mmol) was added dropwise at 0° C., and the resulting mixture was stirred for 30 min followed by the addition of 2-amino pyridine N-oxide (36 mg, 0.327 mmol). The reaction was warmed to rt. After 2 h, the reaction mixture was concentrated, diluted with methanol, and purified by reverse phase HPLC to afford 105 mg (0.167 mmol, 51%) of the title compound. LC/MS: (M+H)+: 629.8.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08901119B2 |
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| 出典データセット | uspto-grants-2014_12 |
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| ORD ID | ord-dcf1187568b94db88d5615ca40736924 |
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| 出典メモ | uspto-grants-2014_12 |
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