反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Into a 250 mL three-necked flask equipped with a magnetic stir bar and nitrogen inlet and outlet were placed 1,1,1-tris{4-[4-(4-aminophenyldiazenyl)phenoxy]phenyl}ethane (Example 5; 0.892 g, 1.00 mmol), phthalic anhydride (0,444 g, 3.00 mmol) and acetic acid (20 mL). The mixture was stirred under refluxing for 14 hours and allowed to cool to room temperature. The precipitate was collected by filtration and dried in an oven to afford 0.96 g (75%) of orange powder, mp >300° C. MS (m/e): 1282 (M+). Anal. Calcd. for C80H51N9O9: C, 74.93%; H, 4.01%; N, 9.83%. Found: C, 75.00%; H, 4.11%; N, 9.44%. 1H-NMR (d6-DMSO, δ in ppm): 2.21 (s, 3H, CCH3), 7.08-7.13 (d, 6H, Ar—H), 7.19-7.21 (dd, 12H, Ar—H), 7.67-7.71 (d, 6H, Ar—H), 7.87-8.03 (m, 24H, Ar—H).
WORKUP
后处理
- customInto a 250 mL three-necked flask equipped with a magnetic stir bar and nitrogen inlet and outlet
- temperatureunder refluxing for 14 hours
- filtrationThe precipitate was collected by filtration
- customdried in an oven