Table 2: Deciding TEA Stoichiometry

Expt No. Moles of MsCl Process Set Point TEA Moles eq HPLC Results Comments
Expt No. 5 1.3 2.2 to 2.35 mole equivalents of TEA. 1.5 93.89% Mesylate,
5.81 % UK
Yield: 87.40%
TEA qty should not be less than optimised qty.
Expt No. 6 1.3 3.0 99.18% Mesylate,
0.81 % carbinol
Yield: 93.33%
No adverse effect on quality of mesylate when excess of TEA was used
Expt No. 7 1.3 2.1 94.66% Mesylate,
4.85 % UK
Yield: 93.33%
Expt No. 8 1.3 2.3 99.22% Mesylate,
0.77% carbinol
Yield: 90.37%