Methyl iodide → HCID 66935892, 화합물
반응식
[O:1]=[C:2]1[CH2:6][CH2:5][N:4]([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[NH:3]1.[C:14](=O)([O-])[O-].[K+].[K+].IC>CN(C=O)C>[CH3:14][N:3]1[C:2](=[O:1])[CH2:6][CH2:5][N:4]1[C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8]참가 물질
5
실험 절차
To a mixture of 1,1-dimethylethyl 3-oxo-1-pyrazolidinecarboxylate (1.00 g, 5.37 mmol) and potassium carbonate (0.89 g, 6.44 mmol) in DMF (10 ml) was added iodomethane (2 M in MTBE, 3.22 ml, 6.44 mmol). The reaction mixture was stirred at rt for 2 h. LCMS indicated completion of the reaction. The mixture was diluted with ethyl acetate/hexanes (1:1, 150 ml) and washed with water (5×50 ml), brine (50 ml), dried (Na2SO4) and concentrated to provide 1,1-dimethylethyl 2-methyl-3-oxo-1-pyrazolidinecarboxylate (0.57 g, 53.0%). LCMS: (M+H)+ 201.0.
후처리
- customcompletion of the reaction
- washwashed with water (5×50 ml), brine (50 ml)
- dry with materialdried (Na2SO4)
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-676b5b01ccc441a4bb1e8ae20a08162d
- 출처 데이터셋
- uspto-grants-2011_02
- 특허 번호
- US07893056B2
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