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% |