Formamide → HCID 22648863, 화합물
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Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[C:7]([CH3:12])[CH:6]=1)=O.[CH:13]([NH2:15])=[O:14]>>[O:14]1[CH:2]=[C:3]([C:5]2[CH:10]=[CH:9][C:8]([OH:11])=[C:7]([CH3:12])[CH:6]=2)[N:15]=[CH:13]1참가 물질
3
실험 절차
A solution of 2-bromo-1-(4-hydroxy-3-methylphenyl)ethanone (200 mg, 0.87 mmol) in formamide (10 mL) was heated to 110° C. for 24 h. The excess formamide was removed by distillation under reduced pressure. The resulting residue was partitioned between a pH 7.0 buffer solution (10 mL) and EtOAc (50 mL). The organic layer was washed with water (10 mL) and brine (10 mL), dried (MgSO4), filtered and concentrated under reduced pressure. The residue was purified by flash chromatography (Hexane:EtOAc, 1:1) to yield the title compound (51 mg, 33% yield).
후처리
- customThe excess formamide was removed by distillation under reduced pressure
- customThe resulting residue was partitioned between a pH 7.0 buffer solution (10 mL) and EtOAc (50 mL)
- washThe organic layer was washed with water (10 mL) and brine (10 mL)
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe residue was purified by flash chromatography (Hexane:EtOAc, 1:1)
출처 및 근거
- ORD 기록
- ord-f61df3abbbf64cc7a48e7f723b7b5a9d
- 출처 데이터셋
- uspto-grants-2004_10
- 특허 번호
- US06806265B2
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