N[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]=[N:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.CCN(C(C)C)[CH:19]([CH3:21])[CH3:20].CC#[N:27]>CN(C=O)C>[NH2:27][C:6]1[CH:5]=[CH:4][C:3]([N:8]=[N:9][C:10]2[CH:15]=[CH:14][C:13]([CH2:20][CH2:19][CH3:21])=[CH:12][CH:11]=2)=[CH:2][CH:7]=1To a solution of the aminoazobenzene (1 eq) and DIPEA (2 eq) in 1:1 MeCN:DMF at 0° C. was added 2-triethylammonium acetic acid chloride chloride8 (1.5 eq) in 1:1 MeCN:DMF and stirred for 15 min, then warmed to ambient temperature and stirred for 1-12 h at which time the solvent was removed in vacuo for purification by reverse phase silica gel chromatography (0.1% formic acid in H2O, gradient up to 50% MeCN: 0.1% formic acid in H2O).
Wird geladen…