Research Article
An Industrial Approach to Production of Tofacitinib Citrate (TFC) as an Anti-COVID-19 Agent: A Joint Experimental and Theoretical Study
Table 3
Optimization of the N-acylation reaction conditions in view of solvents, bases, and temperature.
| | Entry | Catalyst | Solvent | Temperature (°C) | Time (h) | Yield (%) | Type of workup |
| | 1 | K2CO3 | DMF | 50 | 11 | 37.0 | Precipitation | | 2 | TEA | DMF | 50 | 11 | 50.2 | Precipitation | | 3 | TEA | EtOAC | R.T | 11 | 45.0 | Extraction | | 4 | DBU | EtOAC | R.T | 11 | 67.3 | Extraction | | 5 | DBU | Isopropanol | 55 | 17 | 73.5 | Precipitation | | 6 | TEA | Isopropanol | 55 | 17 | 45.0 | Precipitation | | 7 | TEA | Water | 50 | 24 | — | — | | 8 | DBU | Water | 50 | 24 | — | — | | 9 | K2CO3 | Water | 50 | 24 | — | — | | 10 | DBU | — | −10 | 11 | — | — | | 11 | DBU | — | 0 | 11 | — | — | | 12 | DBU | — | R.T | 11 | 93.1 | Precipitation | | 13 | DBU | — | 50 | 11 | 95.6 | Precipitation |
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