Example 8
Spray Drying Compound 5-1
Compound 5-1 was spray dried in a Buchi Mini Spray Dryer model B-290. In the B-290, compound 5-1 was dried co-currently with the drying gas flowing at approximately 30 m3/hr. The B-290's spraying chamber was about 5.5 liters. Therefore, the B-290's average drying residence time was about 0.6 sec. Atomization was achieved by passing nitrogen gas and feed stream through a two fluid nozzle atomizer.
Several drying runs were conducted using different solvents and adjusting the pH. The following table shows the conditions of runs. All runs resulted in an amorphous solid with no change in impurity profile.
Cmpd 5-1InletOutlet
Run #(g)temp (° C.)temp (° C.)Solvent
128 v/w 50:50 EtOH:H2O
22110558 v/w H2O
32110648 v/w 60:40 H2O:EtOH
42100548 v/w 50:50 MeOH:H2O
5270498 v/w MeOH
62100558 v/w 50:50 MeOH:H2O,
XS NaOH
72100578 v/w 50:50 MeOH:H2O
8411065~12 v/w 50:50 MeOH:H2O
9411059~6 v/w 50:50 MeOH:H2O,
XS NaOH
All trials run with N2 flow of ~30 m3/hr, atomization flow of 0.45 m3/hr, and solution feed rate of approx. 5 mL/min
US09868706B2. Processes for the preparation of uracil derivatives (2018-01-16). None [US], Neurocrine Biosciences, Inc. [US]. Inventors: Donald J. Gallagher [US], Laszlo R. Treiber [US], Robert Michael Hughes [US], Onorato Campopiano [US], Peng Wang [US], Yuxin Zhao [US], Shine K. Chou [US], Michael Allen Ouellette [US], Donald Nicholas Hettinger [US].
