[N+:1]([C:4]1[CH:5]=[C:6]([OH:10])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].C(=O)([O-])[O-].[Cs+].[Cs+].[CH3:17][O:18][C:19](=[O:22])[CH2:20]Br.O>CC(C)=O>[CH3:17][O:18][C:19](=[O:22])[CH2:20][O:10][C:6]1[CH:7]=[CH:8][CH:9]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=1Initially charge 50 g (359.4 mmol) of 3-nitrophenol and 175.67 g (539 mmol) of caesium carbonate in 1.0 liter of acetone and add 71.5 g (467.3 mmol) of bromoacetic acid methyl ester. Stir the mixture at 50° C. for 1 h and, after cooling, pour onto 7.5 liters of water. Stir the suspension for 30 min, then filter off with suction and wash the filter residue with water. Dry the solid in a drying cabinet at 50° C. and 100 mbar. 64.3 g (84.7% of theory) of the target compound are obtained.
Wird geladen…
