Methanol → HCID 70224214, 화합물
반응식
[Na].[CH3:2][C:3]1[N+:8]([O-:9])=[C:7]2[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][C:6]2=[C:5]([N+]([O-])=O)[C:4]=1[C:18]([O:20][CH2:21]C)=[O:19].[CH3:23][OH:24]>>[CH3:23][O:24][C:5]1[C:4]([C:18]([O:20][CH3:21])=[O:19])=[C:3]([CH3:2])[N+:8]([O-:9])=[C:7]2[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][C:6]=12참가 물질
실험 절차
In an atmosphere of argon and at room temperature, metallic sodium (86.0 mg, 0.005 g atom) was dissolved in anhydrous methanol (8.0 ml) to which was subsequently added dropwise methanol solution (20.0 ml) of ethyl 2-methyl-4-nitro-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridine-3-carboxylate N-oxide (1.00 g, 3.40 mmol), and the resulting mixture was stirred at room temperature for 29 hours. After evaporation of the solvent under reduced pressure, the resulting residue was mixed with water and extracted with chloroform, and the thus obtained organic layer was washed with water and saturated brine in that order and dried over anhydrous sodium sulfate. After evaporation of the solvent under reduced pressure, the resulting residue was purified by a silica gel column chromatography (ethyl acetate:hexane=5:1—ethyl acetate:methanol=15:1) to obtain the title compound (777.9 mg, 86.3%) as pale yellow powder.
후처리
- customAfter evaporation of the solvent under reduced pressure
- additionthe resulting residue was mixed with water
- extractionextracted with chloroform
- washthe thus obtained organic layer was washed with water and saturated brine in that order
- dry with materialdried over anhydrous sodium sulfate
- customAfter evaporation of the solvent under reduced pressure
- customthe resulting residue was purified by a silica gel column chromatography (ethyl acetate:hexane=5:1—ethyl acetate:methanol=15:1)
출처 및 근거
- ORD 기록
- ord-a7942c820fb646f18a85f27d965caa0b
- 출처 데이터셋
- uspto-grants-2001_07
- 특허 번호
- US06258829B1
반응 노트
불러오는 중…