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. 2023 Jul 10;13(30):20467–20476. doi: 10.1039/d3ra03926a

Conditions for the synthesis of olanzapine derivatives in the reaction of DOLA (1 eq.) : CH3I (1.5 eq.) : K2CO3 or DIPEA (3 eq.) : catalyst (0.01 eq.) in the presence of microwave irradiation (MW) and ultrasound (“)))”).

No. Conditions Temp.a [°C] Pressureb [bar] Solvent/base/catalyst Reaction time [min] Yield [%]
1 MW 147 2.3 DMF/K2CO3/TBAB 2 57
2 MW 150 4.7 DMF/K2CO3/TBAB 1.5 69
3 MW 105 Atm DMF/K2CO3/TBAB 1.5 48
4 MW 150 3.2 DMF//K2CO3/DABCO 1 71
5 MW 150 1.9 DMF/K2CO3/BTBAC 1 69
6 MW 150 2.6 DMF/K2CO3/TEAC 1 73
7 MW 150 2.3 DMF/K2CO3/TMAB 1 72
8 MW 150 2.2 DMF/K2CO3/TEBA 1 87
9 MW 150 2.5 DMF/K2CO3/CTAB 1 95
10 MW 150 0.5 DMF/K2CO3/- 1 38
11 MW 150 0.5 NaDES/K2CO3/TBAB 2 46
12 MW 150 0.5 NaDES/K2CO3/- 2 37
13 MW 150 2.5 NaDES/Glycerine/K2CO3/TBAB 2.5 53
14 ))) 45 Atm DMF/K2CO3/TBAB 120 40
15 ))) 45 Atm DMF/K2CO3/DABCO 120 45
16 ))) 45 Atm DMF/K2CO3/- 120 15
17 ))) 45 Atm NaDES/K2CO3/TBAB 120 25
18 ))) 45 Atm NaDES/DIPEA/TBAB 120 61
a

Highest observed data entered, the maximum temperature was set to 150 °C; reactions in the presence of ultrasound were carried out under reflux, due to the boiling point of CH3I (43 °C).

b

Highest observed data entered, the maximum pressure was set to 10 bar.