OP([O-])(O)=O.[K+].OP([O-])([O-])=O.[K+].[K+].[NH2:14][C:15]1[C:20]([OH:21])=[CH:19][CH:18]=[CH:17][C:16]=1[OH:22].[Cl:23][CH2:24][C:25](Cl)=[O:26]>O>[Cl:23][CH2:24][C:25]([NH:14][C:15]1[C:20]([OH:21])=[CH:19][CH:18]=[CH:17][C:16]=1[OH:22])=[O:26]KH2PO4 (17.2 g, 126.3 mmol) and K2HPO4 (8.2 g, 35.7 mmol) in 188 ml of distilled water were deoxygenated by passing argon through the mixture for 0.5 hour. 2-Aminobenzene-1,3-diol (1 g, 8.0 mmol) was added to the buffer solution and chloroacetyl chloride (0.64 ml, 8.0 mmol) was added slowly to the reaction mixture. After addition was completed, the reaction mixture was stirred at room temperature for 1.5 hours. Water was removed by freeze-drying and the residue was dissolved in 20% MeOH in DCM. The insoluble salt was removed by filtration, the solvent was evaporated to give the subtitled compound which was used without purification in the next step.
Wird geladen…
