Dimethylacetamide → HCID 178457235、化合物
反応式
[C:1]([O:5][C:6]([N:8]([CH3:23])[C@H:9]1[CH2:14][CH2:13][C@H:12]([C:15]#[C:16][CH2:17]OS(C)(=O)=O)[CH2:11][CH2:10]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH2:24]([CH2:27][NH2:28])[CH:25]=C.[CH3:29]C(N(C)C)=O>>[C:1]([O:5][C:6](=[O:7])[N:8]([C@H:9]1[CH2:14][CH2:13][C@H:12]([C:15]#[C:16][CH2:17][N:28]([CH2:27][CH:24]=[CH2:25])[CH3:29])[CH2:11][CH2:10]1)[CH3:23])([CH3:4])([CH3:3])[CH3:2]参加物
4
実験手順
A solution of 420 mg (1.22 mmol) of trans-Methanesulfonic acid 3-[4-(tert-butoxycarbonyl-methyl-amino)-cyclohexyl]-prop-2-ynyl ester in 4 ml DMA was treated at 0° C. with 0.234 ml (2.43 mmol) of N-allylmethylamine and stirred at RT for 16 h. The solution was concentrated and the residual oil was extracted with aqueous sat. NaHCO3/Et2O (3×). The organic phases were washed with aqueous 10% NaCl solution and dried over Na2SO4 to yield after flash column chromatography on silica gel with hexane/EtOAc (2:1) 355 mg (91%) trans-{4-[3-(Allyl-methyl-amino)-prop-1-ynyl]-cyclohexyl}-methyl-carbamic acid tert-butyl ester, MS: 321 (MH+).