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HRID 63992作成日:2026年10月23日
1-Pyrrolidinecarboxylic acid, 2-oxo-, 1,1-dimethylethyl ester → tert-butyl N-[4-(3-fluorophenyl)-4-oxobutyl]carbamate
https://huagongshe.com/ja/reaction/63992
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Pyrrolidinecarboxylic acid, 2-oxo-, 1,1-dimethylethyl ester | HCID 379000 | — |
| 反応物 | HCID 178505773 | HCID 178505773 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | tert-butyl N-[4-(3-fluorophenyl)-4-oxobutyl]carbamate | HCID 67330612 | — |
反応手順
In a round-bottomed flask was charged tert-butyl 2-oxopyrrolidine-1-carboxylate (2.2 g, 11.9 mmol) and THF (25 mL). The mixture was cooled down to −78° C. first, followed by slow addition of (3-fluorophenyl)magnesium bromide (17.8 mL, 17.8 mmol, 1.0 M solution in THF) over 15 minutes. The mixture was stirred for 3 hours, during which time the bath temperature rose from −78° C. to −10° C. The reaction was quenched by drop-wise addition of 1N HCl (2 mL) and warmed up to ambient temperature, followed by addition of EtOAc and water. After separating the organic layer, the aqueous layer was extracted with EtOAc three times. The combined organic layers was dried over Na2SO4 and concentrated to yield the product as a clear oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09447104B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-0e0d6802bbec4410b6ba92c729e66ce8 |
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| 出典メモ | uspto-grants-2016_09 |
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