O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.O=P(Cl)(Cl)Cl.[CH3:20][C:21]([C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)([CH3:32])[CH2:22][NH:23][C:24](=O)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1>C1(C)C(C)=CC=CC=1>[CH3:20][C:21]1([CH3:32])[C:33]2[C:38](=[CH:37][CH:36]=[CH:35][CH:34]=2)[C:24]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[N:23][CH2:22]11.42 g (10.0 mmol) of P2O5 and POCl3 (4 ml) were added to a solution of 1.27 g (5.0 mmol) of N-(2-methyl-2-phenylpropyl)benzamide in xylene (20 ml) and the mixture was heated at 150° C. for 3 h. After cooling to RT the mixture was concentrated to small volume under vacuum. The residue was made alkaline with a 20% aqueous NaOH solution. It was then extracted with EE and the organic phase was dried over Na2SO4, filtered and concentrated to small volume under vacuum. 634 mg (2.7 mmol) of 4,4-dimethyl-1-phenyl-3,4-dihydroisoquinoline were obtained as the residue, which was reacted further with no additional purification.
Wird geladen…
