참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylsilane | HCID 12052 | — |
| 반응물 | N-[5-Chloro-4-(2-chloro-acetyl)-2-methyl-phenyl]-acetamide | HCID 21963317 | — |
| 용매 | Trifluoroacetic acid | HCID 6422 | — |
| 생성물 | N-[5-Chloro-4-(2-chloro-ethyl)-2-methyl-phenyl]-acetamide | HCID 21963171 | 88.2% |
반응 단계
To a solution of N-[5-Chloro-4-(2-chloro-acetyl)-2-methyl-phenyl]-acetamide (10 g, 38.44 mmol) in trifluoroacetic acid (100 mL) at <20° C. was added portionwise, triethylsilane (15.35 mL, 96.1 mmol). The reaction was heated to 60° C. and stirred overnight. The reaction was cooled to rt and poured over ice/H2O and stirred for 30 min as a grey precipitate formed. The precipitate was collected by filtration and dried in vacuo overnight to give desired product (8.35 g, 33.92 mmol). Yield=88%; MS (APCI): 246 [M+H]+. 1H NMR (400 MHz, CDCl3) δ 7.89 (s, 1H), 7.05 (s, 1H), 6.93 (bs, 1H, NH), 3.69 (t, J=7.26 Hz, 2H), 3.10 (t, J=7.26 Hz, 2H), 2.20 (d, J=4.48 Hz, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07101886B2 |
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| 출처 데이터셋 | uspto-grants-2006_09 |
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| ORD ID | ord-731ee461f91146d2852063712cd16c60 |
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| 출처 메모 | uspto-grants-2006_09 |
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