참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Formic Acid | HCID 284 | — |
| 반응물 | Acetic Anhydride | HCID 7918 | — |
| 반응물 | 2-Chloro-3-fluoroaniline | HCID 88884 | — |
| 생성물 | N-(2-Chloro-3-fluorophenyl)formamide | HCID 57346568 | 95.1% |
반응 단계
A solution of acetic anhydride (10 mL, 106 mmol) and formic acid (30 mL, 795 mmol) was stirred at room temperature for 10 mins. 2-Chloro-3-fluoroaniline (2.9 g, 20 mmol) was added and the reaction mixture was stirred at 60° C. for 1.5 h. After cooling to room temperature, the solvents were removed in vacuo and the residue was redissolved in DCM (100 mL) and was washed with sat aq. NaHCO3 until the aqueous phase had a measured pH of 8. The organic layer was further washed with water (2×100 mL), separated and dried over MgSO4. Filtration and concentration in vacuo gave N-(2-chloro-3-fluoro-phenyl)-formamide (3.3 g, 95%) as a colorless solid which did not require further purification. MS (M+H)+: 173.9, tR=2.04 min (method 1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08084614B2 |
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| 출처 데이터셋 | uspto-grants-2011_12 |
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| ORD ID | ord-2f1da52840a449cb8d6cbfcb5e7d9ad6 |
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| 출처 메모 | uspto-grants-2011_12 |
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