化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → [(2S,4EZ)-1-(biphenyl-4-ylcarbonyl)-4-(methoxyimino)pyrrolidin-2-yl] acetic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | O-methylhydroxylammonium chloride | HCID 11639 | — |
| 反応物 | [(2s)-1-(Biphenyl-4-ylcarbonyl)-4-oxopyrrolidin-2-yl]acetic acid | HCID 69036428 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | [(2S,4EZ)-1-(biphenyl-4-ylcarbonyl)-4-(methoxyimino)pyrrolidin-2-yl] acetic acid | HCID 131727525 | 48.7% |
反応手順
A solution of [(2S)-1-(biphenyl-4-ylcarbonyl)-4-oxopyrrolidin-2-yl]acetic acid (Intermediate 5, 1.50 g, 6.64 mmol), hydroxylamine methyl ether hydrochloride (0.58 g, 6.96 mmol) and triethylamine (1.62 ml, 11.60 mmol) in chloroforme (30 ml) was stirred at RT for 2 days Solvent was removed under reduced pressure and the residue was taken up in ethyl acetate. Organic phase was washed twice with a solution of citric acid 10% and once with brine. Organic phase was then dried on MgSO4, filtered, and concentrated to give [(2S,4EZ)-1-(biphenyl-4-ylcarbonyl)-4-(methoxyimino)pyrrolidin-2-yl]acetic acid as a cream solid (1.14 g). Yield: 45%. HLPC purity: 92%
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07557136B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-5a0a347e841840a688139dd8ff711e73 |
| 出典メモ | uspto-grants-2009_07 |