Table 1: Deciding Reagent Stoichiometry

Expt. No. Solvent Volumes Process Set Point MsCl Moles eq HPLC Results Comments
Expt No. 1 10 volume 1.25 - 1.35 mole equivalents of MsCl. 1.1 98.09% Mesylate,
1.23 % carbinol
Yield: 97.9%
Expt No. 2 10 volume 2.0 98 A2% Mesylate,
0.15 % carbinol
Yield: 57.7%
Expt No. 3 10 volume 1.0 91.97% Mesylate,
5.78 % carbinol
Yield: 94.81%
Expt No. 4 10 volume 1.5 98.96% Mesylate, 0.7% carbinol Yield: 90.37%