関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pentanoic Acid | HCID 7991 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Pivaloyl chloride | HCID 62493 | — |
| 反応物 | Lithium Chloride | HCID 433294 | — |
| 反応物 | 4-Methyl-5-phenyl-2-oxazolidinone, (4S,5R)- | HCID 853161 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (4S,5R)-4-Methyl-3-pentanoyl-5-phenyl-oxazolidin-2-one | HCID 69269495 | — |
反応手順
To a 0° C. stirred solution of valeric acid (3.83 mL, 35.2 mmol) and Et3N (14.7 mL, 106 mmol) in dry THF (175 mL) was added trimethylacetyl chloride (5.29 mL, 42.3 mmol) dropwise. The mixture was stirred at 0° C. for 1 hour and (4S,5R)-(−)-4-methyl-5-phenyl-2-oxazolidinone (7.50 g, 42.3 mmol) was added followed by LiCl (1.79 g, 42.3 mmol). The reaction was warmed to room temperature overnight with good stirring. The mixture was filtered and the filtrate was concentrated under reduced pressure. Et2O (75 mL) was added to the residue, which was washed with sat. NaHCO3 (3×40 mL), 1N HCl (3×40 mL), and brine (2×40 mL). The organic phase was dried over MgSO4, filtered and concentrated under reduced pressure to give a quantitative yield of crude product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07388023B2 |
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| 出典データセット | uspto-grants-2008_06 |
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| ORD ID | ord-17bf84a0f9ce45c9bc7ffc3dad778df2 |
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| 出典メモ | uspto-grants-2008_06 |
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