The document summarizes experiments using a Gas Module attached to an H-Cube Pro reactor to enable gas-liquid and gas-solid reactions. Key findings include: 1) The Gas Module allows versatile use of various gases including oxygen, carbon monoxide, ethylene and others for reactions. 2) Reactions with gases are fast, completing in under 10 minutes, and the Gas Module is capable of pressures up to 100 bar. 3) Optimization of alcohol oxidation over different catalysts and conditions showed the highest conversion and selectivity at 100°C, 100 bar, and 5% Ru/Al2O3 catalyst. 4) Aminocarbonylation reactions achieved up to 82% conversion using different

1. Gas Module:
Reactions With
Other Gases

2. Gas Module
• Versatile:
Compressed Air, O2, CO, C2H4, SynGas,
CH4, C2H6, He, N2, N2O, NO, Ar.
• Fast:
Reactions with other gases complete in
less than 10 minutes
• Powerful:
Up to 100 bar capability.
• Robust:
All high quality stainless steel parts.
• Simple:
3 button stand-alone control or via simple
touch screen control on H-Cube Pro™.

3. Use of Gas Module Attached to the H-Cube Pro™
Gas Module HPLC pump H-Cube Pro™
Filter included Check valve
included

4. Chemical Production and E-Factors in Industry

5. Problems with Oxidation

6. Alcohol oxidation: Optimization
Temp.
Pressure (oC) CatCart Conversion Selectivity
40 25 1 % Au/TiO2 0 –
40 65 1 % Au/TiO2 6.5 >85
1%
40 25 Au/Fe2O3 0 –
General conditions: H-Cube Pro with Gas 1%
Module, 50 mL/min oxygen gas, 1 mL/min liquid 40 65 Au/Fe2O3 12.7 0
flow rate (0.05M in acetone, 20 mL sample 5%
volume), CatCart: 70mm., 1 % Au/TiO2 (cartridge: 40 25 Ru/Al2O3 2.8 ~100
70mm, THS 01639), 5%
40 65 Ru/Al2O3 3.6 ~100
5%
Very fast addition of alcohol to gold surface. 100 65 Ru/Al2O3 2.7 ~100
Alkoxide formation.
5%
100 100 Ru/Al2O3 8.5 ~100
5%
100 140 Ru/Al2O3 15.5 ~100
100 65 1 % Au/TiO2 5.6 84
Batch ref.: Oxygen; perruthenate modified 100 100 1 % Au/TiO2 47.2 93
mesoporous silicate MCM-41 in toluene
1%
T=80°C; 24 h; Bleloch, Andrew; et al. Chemical 100 140 Au/TiO2 ~100 93
Communications, 1999 , 8,1907 - 1908
1%
100 65 Au/Fe2O3 4 0
1%
100 100 Au/Fe2O3 31 7
100 • Area% of desired product in GC-MS / (100 – Area% of reactant in GC-

7. Aromatization of heterocycles
Reaction parameters were tested:
- H-Cube Pro with and without GasModule
- Oxidizing agent: Hydrogen-peroxide and Oxygen
- Catalyst: MnO2, Amerlyst 36, Au/TiO2
- Solvent: Acetone/H2O2, Acetone
- Temperature 60-150oC, pressure 20-50 bar, flow rate 1 ml/min, concentration: 0.05 mmol/ml
Oxidizing Temperature Pressure
agent Solvent Catalyst (oC) (bar) Conversion Comment
MnO2 Acetone MnO2 60 20 82% Blockage after 10 minutes
Acetone - H2O2 (4- 68% after 1 run
H2O2 1) Au/TiO2 70 20 78% after 2 run
Acetone - H2O2 (4- 68% after 1 run The catalyst was reactivated
H2O2 1) Au/TiO2 100 30 98% after 2 run with H2O2 between the runs.
O2 (10 ml/min) Acetone Au/TiO2 75 11 8%
After 10 minutes the
conversion was dropped to
O2 (10 ml/min) Acetone Au/TiO2 150 11 95% 50%
O2 (50 ml/min) Acetone Au/TiO2 150 20 > 98%

8. Aminocarbonylation
 Conditions: 100oC, 30 bar, CO gas, 0.5 ml/min liquid flow rate, 0.01 M in THF
 Catalyst: Polymer supported Pd(PPh3)4
 Reference test was managed on X-Cube
 Reaction was repeated
 Different gas flow rates were tested
Results
HC-Pro with gas module (CO flow rate)
Reaction 10 30 60 30 30 60 60 60 XC
ml/min ml/min ml/min ml/min ml/min ml/min ml/min ml/min reference
Conversion
% 60 65 79 66 62 79 79 82 0