[C:1]([O:4][C:5]1[CH:17]=[CH:16][C:15]2[C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[CH2:8][C:7]=2[CH:6]=1)(=[O:3])[CH3:2].C(O)(=O)C.C(OC(=O)C)(=O)C.[Br:29]Br>O>[Br:29][C:11]1[CH:12]=[CH:13][C:14]2[C:15]3[C:7](=[CH:6][C:5]([O:4][C:1](=[O:3])[CH3:2])=[CH:17][CH:16]=3)[CH2:8][C:9]=2[CH:10]=12-Acetoxyfluorene (70 g) was added to a mixture of acetic acid (330 mL) and acetic anhydride (110 mL) and heated up to 65° C. to obtain a homogeneous solution. Bromine (125 g) was dropwise added thereto in 40 minutes and stirred for further one hour. The reaction solution was poured into water (1 L) to obtain deposited crystals by filtration under reduced pressure. The dried crystals were ecrystallized from a mixed solution of ethanol (400 mL) and ethyl acetate (300 mL) to obtain colorless needle-shaped 2-bromo-7-acetoxyfluorene (69 g). The melting point of this compound was 130° C.
Wird geladen…
