[CH3:1][C:2]([C:5]1[CH:26]=[CH:25][C:8]([C:9]([NH:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][CH2:19][C:20](OCC)=[O:21])=[CH:14][CH:13]=2)=[O:10])=[CH:7][CH:6]=1)([CH3:4])[CH3:3].[H-].[Al+3].[Li+].[H-].[H-].[H-].C(OCC)C.S(=O)(=O)(O)O>O>[CH3:4][C:2]([C:5]1[CH:26]=[CH:25][C:8]([C:9]([NH:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][CH2:19][CH2:20][OH:21])=[CH:14][CH:13]=2)=[O:10])=[CH:7][CH:6]=1)([CH3:1])[CH3:3]2.2 g. of the compound of Example 31 are reduced with 0.65 g. lithium aluminum hydride in 50 ml. boiling diethyl ether. The reaction mixture is mixed with water, sufficient 10% sulphuric acid is added thereto just to dissolve the precipitate, extracted with diethyl ether, evaporated to dryness and the remaining oil purified by column chromatography (silica gel; dichloromethane/methanol 99:1 v/v). The appropriate fractions are evaporated to dryness in a vacuum, the residue is first recrystallised from ethyl acetate/ligroin (1:1 v/v) and then from toluene to give 0.6 g. (31% of theory) of the title compound; m.p. 136°-142° C.
Wird geladen…
