참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Chloroacetanilide | HCID 11485 | — |
| 반응물 | Monobasic potassium phosphate | HCID 516951 | — |
| 반응물 | 2-Amino-1-(3-bromophenyl)ethan-1-ol | HCID 22021067 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 2-[2-(3-bromo-phenyl)-2-hydroxy-ethylamino]-N-phenyl-acetamide | HCID 67000657 | 42.3% |
반응 단계
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)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08063088B2 |
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| 출처 데이터셋 | uspto-grants-2011_11 |
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| ORD ID | ord-e54f51f2b32547079b951d7506d0e604 |
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| 출처 메모 | uspto-grants-2011_11 |
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