[CH3:1][C:2]1[C:7]([CH2:8][C:9]#[N:10])=[CH:6][CH:5]=[CH:4][N:3]=1.[CH2:11]([OH:13])[CH3:12].[ClH:14]>C(Cl)Cl>[ClH:14].[CH3:1][C:2]1[C:7]([CH2:8][C:9](=[NH:10])[O:13][CH2:11][CH3:12])=[CH:6][CH:5]=[CH:4][N:3]=1Through a stirred solution of Example 53A (1.7 g, 12.86 mmol), absolute ethanol (0.89 g, 19.35 mmol) and anhydrous methylene chloride (25 ml) was bubbled with hydrogen chloride gas for 20 min. The mixture was allowed to stand overnight in the refrigerator. The product was precipitated with anhydrous ether and filtered to obtain the title compound, which was immediately used in the next step. MS (ESI+) m/z 180 (M+H)+.
Wird geladen…