Methanol → HCID 66936493、化合物
反応式
[CH3:1][N:2]1[C:6](=O)[CH2:5][CH2:4][N:3]1[C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9].CO>ClCCl>[CH3:1][N:2]1[CH2:6][CH2:5][CH2:4][N:3]1[C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9]参加物
4
実験手順
To a solution of 1,1-dimethylethyl 2-methyl-3-oxo-1-pyrazolidinecarboxylate (0.98 g, 4.89 mmol) in dry dichloromethane was added borane dimethyl sulfide complex (1.16 ml, 12.24 mmol). The mixture was stirred at rt overnight. LCMS indicated ˜40% starting material left. Another portion of borane dimethyl sulfide complex (0.5 ml, 5.28 mmol) was added, and stirring continued overnight. Methanol was added dropwise to the reaction mixture until bubbling ceased. Water (1 ml) was then added, and the mixture was refluxed for 1 h. After cooling to rt, the mixture was concentrated to dryness under vacuum. The residue was taken up in water (30 ml) and dichloromethane (45 ml), the organic layer was separated, and the aqueous layer was extracted with dichloromethane (45 ml). The combined organic solution was dried (Na2SO4), filtered and concentrated to provide 1,1-dimethylethyl 2-methyl-1-pyrazolidinecarboxylate (0.48 g, 52.7%). LCMS: (2M+H)+ 372.9.