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. 2023 Nov 20;13(48):33566–33587. doi: 10.1039/d3ra06560j

Effects of various factors on the synthesis of 4aa.

graphic file with name d3ra06560j-u1.jpg
Entry Nanocatalyst (g) Conditions Solvent (3 mL) Time (min) Yieldb (%)
1 Grinding, r.t. 30 Trace
2 80 °C 180 Trace
3 0.005 Grinding, r.t. 30 25
4 0.007 Grinding, r.t. 30 32
5 0.01 Grinding, r.t. 20 37
6 0.03 Grinding, r.t. 20 45
7 0.05 Grinding, r.t. 20 91
8 0.07 Grinding, r.t. 15 95
9 0.09 Grinding, r.t. 15 90
10 0.1 Grinding, r.t. 15 88
11 0.07 Reflux EtOH 4 h 55
12 0.07 Reflux EtOH/H2O (1 : 1) 3 h 60
13 0.07 Reflux H2O 7 h 20
14 0.07 Reflux Toluene 5 h 30
15 0.07 Reflux Chloroform 5 h 12
a

Reaction conditions: benzaldehyde (1 mmol), dimedone (1 mmol), malononitrile (1 mmol), catalysts, under different conditions.

b

Isolated pure yield.