Sodium Carbonate → 7-Fluoro-3-methyl-2,3-dihydro-4H-1,3-benzoxazin-4-one
반응식
[F:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([NH:8][CH3:9])=[O:7])=[C:4]([OH:12])[CH:3]=1.[C:13](=O)([O-])[O-].[Na+].[Na+]>C=O.C(O)=O>[F:1][C:2]1[CH:11]=[CH:10][C:5]2[C:6](=[O:7])[N:8]([CH3:13])[CH2:9][O:12][C:4]=2[CH:3]=1참가 물질
5
실험 절차
A mixture of 4-fluoro-2-hydroxy-N-methyl-benzamide (0.3 g, 1.77 mmol) in formaldehyde (37% aq. soln) (2 mL) and formic acid (2 mL) was refluxed for 1 hour then poured onto ice. The mixture was neutralised with sodium carbonate and extracted into chloroform (3×30 mL). The combined organics were dried (MgSO4), and reduced in vacuo to give a white solid which was chromatographed on silica, eluting with 10-50% ethyl acetate in isohexane to give the desired compound as a white solid (0.24 g).
후처리
- temperaturewas refluxed for 1 hour
- additionthen poured onto ice
- extractionextracted into chloroform (3×30 mL)
- dry with materialThe combined organics were dried (MgSO4)
- customto give a white solid which
- customwas chromatographed on silica
- washeluting with 10-50% ethyl acetate in isohexane
출처 및 근거
- ORD 기록
- ord-3a14f44bd2bd48a2a3cdf00f41c69cd9
- 출처 데이터셋
- uspto-grants-2011_05
- 특허 번호
- US07943607B2
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