関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | (RS)-4-{4-[3-(4-chloro-phenyl)-ureido]-phenyl}-2,2-dimethyl-oxazolidine-3-carboxylic acid tert-butyl ester | HCID 67151498 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Tetrahydrofuran ethyl acetate | HCID 21939870 | — |
| 生成物 | HCID 67151552 | HCID 67151552 | 133.7% |
反応手順
To a solution of (RS)-4-{4-[3-(4-chloro-phenyl)-ureido]-phenyl}-2,2-dimethyl-oxazolidine-3-carboxylic acid tert-butyl ester (0.24 g) in acetonitrile (3 ml) were added water (9 ml) and trifluoroacetic acid (0.33 ml). The mixture was heated overnight at 80° C. The mixture was then cooled to room temperature and diluted with ethyl acetate/THF (1:1). The resulting mixture was washed sequentially with 1 N aq. sodium hydroxide solution and saturated brine, the phases were then separated and the organic phase was dried over sodium sulphate and concentrated in vacuo to afford (RS)-1-[4-(1-amino-2-hydroxy-ethyl)-phenyl]-3-(4-chloro-phenyl)-urea (0.22 g, quant.) an off-white solid. MS (ISP): 291.1 ([{37Cl}M+H—OH]+), 289.1 ([{35Cl}M+H—OH]+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08354441B2 |
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| 出典データセット | uspto-grants-2013_01 |
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| ORD ID | ord-afa0ac61f4034c7caa071242fcf579de |
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| 出典メモ | uspto-grants-2013_01 |
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