反応 #64268

反応方程式

toluene

4-aminophenol

4-phenylethynyl-4'-fluorobenzophenone

potassium carbonate

→

desired product

収率 85.0%

4-(4-Aminophenoxy)-4'-phenylethynylbenzophenone

収率 85.0%

溶媒

DMAc

water

反応条件

後処理

1. 1
   その他In a 250 mL flask equipped with nitrogen inlet
2. 2
   温度Dean-Stark trap, and reflux condenser
3. 3
   温度cooled to room temperature
4. 4
   ろ過the resulting light yellow powder was collected by filtration
5. 5
   その他Recrystallization from toluene

実験手順

In a 250 mL flask equipped with nitrogen inlet, overhead stirring assembly, Dean-Stark trap, and reflux condenser were placed 4-aminophenol (5.46 g, 0.05 mol), 4-phenylethynyl-4'-fluorobenzophenone (15.02 g, 0.05 mol), potassium carbonate (7.6 g, 0.055 mol), toluene (20 mL), and DMAc (45 mL). The mixture was heated to 150° C. for 2 h, then cooled to room temperature. The reaction mixture was poured into water and the resulting light yellow powder was collected by filtration. Recrystallization from toluene afforded the desired product in 85% yield: m.p. 151°-153° C. IR (KBr); 3382 and 3314 cm-1 (NH2); 3049, 1599, and 1509 cm-1 (aromatic C--H); 2217 cm-1 (C=C); and 1645 cm-1 (C=O): Mass Spec. m/e (relative intensity): M+, 389.4 (100); FW=389.44 g/mol.

出典