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Trimethylsilyldiazomethane → methyl 3-[(2R,4EZ)-1-(biphenyl-4-ylcarbonyl)-4-(methoxyimino)pyrrolidin-2-yl]propanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trimethylsilyldiazomethane | HCID 167693 | — |
| 反応物 | 3-[(2R,4EZ)-1-(biphenyl-4-ylcarbonyl)-4-(methoxyimino)pyrrolidin-2-yl]propanoic acid | HCID 131727528 | — |
| 溶媒 | 2-Methylbenzyl alcohol | HCID 6994 | — |
| 生成物 | methyl 3-[(2R,4EZ)-1-(biphenyl-4-ylcarbonyl)-4-(methoxyimino)pyrrolidin-2-yl]propanoate | HCID 131727527 | 96% |
反応手順
To a solution of 3-[(2R,4EZ)-1-(biphenyl-4-ylcarbonyl)-4-(methoxyimino)pyrrolidin-2-yl]propanoic acid (Intermediate 8, 20 mg, 0.05 mmol) in toluene-methanol (1 ml, 3-1) was added (diazomethyl)trimethylsilane (0.110 ml, 2M in hexane). After 3 hours, the reaction mixture was concentrated and purified by silica gel column chromatography (ethyl acetate) to give methyl 3-[(2R,4EZ)-1-(biphenyl-4-ylcarbonyl)-4-(methoxyimino)pyrrolidin-2-yl]propanoate (20 mg). Yield: 96%. HPLC purity: 94%
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-9a97026e02ac4b98842f0e341208e0bf |
| 出典メモ | uspto-grants-2009_07 |