関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Chloroacetanilide | HCID 11485 | — |
| 反応物 | Monobasic potassium phosphate | HCID 516951 | — |
| 反応物 | 2-Amino-1-(3-bromophenyl)ethan-1-ol | HCID 22021067 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-[2-(3-bromo-phenyl)-2-hydroxy-ethylamino]-N-phenyl-acetamide | HCID 67000657 | 42.3% |
反応手順
To a solution of 2-amino-1-(3-bromo-phenyl)-ethanol (example 33, step 1, 1.34 g) and crude 2-chloro-N-phenyl-acetamide (example 33, step 2, 1.0 g) in acetonitrile (15 mL) was added potassium carbonate (1.03 g). The mixture was heated to 80° C. overnight. A 1M solution of KH2PO4 was added, followed by ethyl acetate. The phases were separated, and the inorganic one was extracted with ethyl acetate (x2). The combined organic layers were washed with brine, dried (Na2SO4) and concentrated in vacuo. Column chromatography (SiO2, CH2Cl2/MeOH 95:5) followed by precipitation from a mixture of diethylether/n-heptane (1:4) gave 2-[2-(3-bromo-phenyl)-2-hydroxy-ethylamino]-N-phenyl-acetamide (0.87 g, 42%) as a white solid, MS: 349.1 (M+H, 1Br)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08063088B2 |
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| 出典データセット | uspto-grants-2011_11 |
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| ORD ID | ord-e54f51f2b32547079b951d7506d0e604 |
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| 出典メモ | uspto-grants-2011_11 |
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