関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | (R)-1-[4-(4-fluoro-benzyloxy)-phenyl]-5-oxo-pyrrolidine-3-carboxylic acid methyl ester | HCID 68614773 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | (R)-1-[4-(4-fluoro-benzyloxy)-phenyl]-5-oxo-pyrrolidine-3-carboxylic acid | HCID 40802443 | 51.2% |
反応手順
A solution of 1.27 g (3.7 mmol) of (R)-1-[4-(4-fluoro-benzyloxy)-phenyl]-5-oxo-pyrrolidine-3-carboxylic acid methyl ester in 77 ml of dioxane is treated with 8.64 ml of hydrochloric acid (37%). The mixture is heated at 52° C. for 18 h in a closed flask. For the working-up, the solution is evaporated under reduced pressure to yield the crude acid as a yellowish solid. For purification, the crude acid is triturated at −5° C. in 10 ml of ethyl acetate. The solid is collected on a filter funnel and then dried under high vacuum to yield 0.624 g (51% of theory) of (R)-1-[4-(4-fluoro-benzyloxy)-phenyl]-5-oxo-pyrrolidine-3-carboxylic acid as a white solid; MS: m/e=330 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07122562B2 |
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| 出典データセット | uspto-grants-2006_10 |
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| ORD ID | ord-4c4a70b058ae4ded8f20a9ec6f2d3b9b |
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| 出典メモ | uspto-grants-2006_10 |
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