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Table 1 Optimization of reaction conditions

From: A green and facile synthesis of an industrially important quaternary heterocyclic intermediates for baricitinib

Entry Solvent Temperature (°C) Time V-5/V-5-2 (mol/mol)
1 DCM 5 30 min 76.0/24.0
2 DCM 0 30 min 90.9/9.1
3 DCM − 5 30 min 95.7/4.3
4 DCM − 10 30 min 97.6/2.4
5 DCM − 15 1.5 h 97.1/2.9