Potassium Carbonate → 3-oxo-3,4-dihydro-2H-1,4-benzoxazine-6-carbaldehyde
반응식
Cl[CH2:2][C:3]([NH:5][C:6]1[CH:7]=[C:8]([CH:11]=[CH:12][C:13]=1[OH:14])[CH:9]=[O:10])=[O:4].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[O:4]=[C:3]1[NH:5][C:6]2[CH:7]=[C:8]([CH:9]=[O:10])[CH:11]=[CH:12][C:13]=2[O:14][CH2:2]1참가 물질
4
실험 절차
3-(Chloroacetylamino)-4-hydroxy-benzaldehyde (2.4 g, 13.2 mmol) and potassium carbonate (9.1 g, 66.1 mmol) are stirred at room temperature in 50 mL of acetonitrile for 12 hours. The acetonitrile is evaporated and the residue is taken up in 50 mL of water. After standing at room temperature for 10 minutes, the precipitate is collected by filtration and recrystallized from ethyl acetate to give 1.4 g (60% yield) of 3-oxo-3,4-dihydro-2H-benzo[1,4]oxazine-6-carbaldehyde; mp 220-222° C.
후처리
- customThe acetonitrile is evaporated
- filtrationthe precipitate is collected by filtration
- customrecrystallized from ethyl acetate
출처 및 근거
- ORD 기록
- ord-7b53db98cf2f441ba191a2e606e1983f
- 출처 데이터셋
- uspto-grants-2001_01
- 특허 번호
- US06177422B1
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