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A 50 mL Hastelloy 27 6C high pressure autoclave was fitted with an impeller, gas inlet tube, sample tube, and thermowell. The autoclave was heated with a heating block, with tempera- 5 ture control provided by feedback via a thermocouple in the autoclave thermowell. Pure carbon monoxide gas (>99.9%) was fed to the autoclave via a high pressure regulator. The autoclave was charged with 20% W-heteropoly/silica catalyst (1.48 g) propionic acid (12.28 g, 0.16 mo!) and MDP (14.1 g, 0.08 mo!) and water (1.4 g, 0.08 mo!) and sealed. The auto› clave was secured to the stand and the system was pressurized with 200 psig nitrogen and vented. This purging procedure was repeated two times. The autoclave was then purged with carbon monoxide and pressurized to 200 psig carbon mon- 15 oxide. The temperature in the autoclave was increased to 140° C. Upon reaching 140° C., the pressure in the autoclave was increased to 1,000 psig carbon monoxide. The reaction was held at these conditions for 2 hours and then cooled to room temperature and vented. Finally the autoclave was purged with nitrogen and unloaded. The reaction contents were ana› lyzed by GC. Results are shown in Table 12. 

The procedure of Example 67 was repeated using either MDP/propionic acid or MDA/acetic acid and water at target equivalents of 1 eq. of MDA(MDP), 2 eq. acetic (propionic) acid, and 1 eq. water at a reaction pressure ofl 000 psig carbon monoxide. The examples were run with the solid catalyst and corresponding loading, at the temperature, and for the hold› ing time shown in Table 12. Calculated yields are also given in Table 12. 

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## Example 67 

## Examples 68-83 

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A 50 mL Hastelloy 276C high pressure autoclave was fitted with an impeller, gas inlet tube, sample tube, and thermowell. The autoclave was heated with a heating block, with tempera› ture control provided by feedback via a thermocouple in the autoclave thermowell. Pure carbon monoxide gas (>99.9%) was fed to the autoclave via a high pressure regulator. The autoclave was charged with AMBERLYST 36 D catalyst (1.43 g), propionic acid (12.3 g, 0.166 mo!), MDP (14.1 g, 0.088 mo!), and water (1.5 g, 0.083 mo!) and sealed. The autoclave was secured to the stand and the system was pres› surized with 200 psig nitrogen and vented. This purging pro› cedure was repeated two times. The autoclave was then purged with carbon monoxide and pressurized to 500 psig carbon monoxide. The temperature in the autoclave was increased to 140° C. Upon reaching 140° C., the pressure in the autoclave was increased to 1,000 psig carbon monoxide. The reaction was held at these conditions for 2 hours and then cooled to room temperature and vented. Finally the autoclave was purged with nitrogen and unloaded. The reaction con- tents were analyzed by GC. The results are shown in Table 13. 

Example 84 was repeated with the catalyst and catalyst loading and amount of propionic acid and water given in Table 13. Each reaction was run at 1000 psig carbon monox- ide and at the temperature and for the time indicated in Table 13. Yield to desired products and selectivity are also given in Table 13. 

## Examples 84 

## Examples 85-91 

