Reaction #816383

ord-105bc92990b24b3d9a6b481443a8c1a0

Reaction equation

O=C=Nc1ccc(Cc2ccc(N=C=O)cc2)cc1
pMDI
CC(C)C[C@H]1C(=O)N2CCC[C@H]2[C@]2(O)O[C@](NC(=O)[C@@H]3C=C4c5cccc6[nH]c(Br)c(c56)C[C@H]4N(C)C3)(C(C)C)C(=O)N12.CS(=O)(=O)O
bromocriptine
CC(C)C[C@H]1C(=O)N2CCC[C@H]2[C@]2(O)O[C@](NC(=O)[C@@H]3C=C4c5cccc6[nH]c(Br)c(c56)C[C@H]4N(C)C3)(C(C)C)C(=O)N12.CS(=O)(=O)O
bromocriptine mesylate
→
CC(C)C[C@H]1C(=O)N2CCC[C@H]2[C@]2(O)O[C@](NC(=O)[C@@H]3C=C4c5cccc6[nH]c(Br)c(c56)C[C@H]4N(C)C3)(C(C)C)C(=O)N12
Bromocriptine

Reactants

O=C=Nc1ccc(Cc2ccc(N=C=O)cc2)cc1
pMDI
CC(C)C[C@H]1C(=O)N2CCC[C@H]2[C@]2(O)O[C@](NC(=O)[C@@H]3C=C4c5cccc6[nH]c(Br)c(c56)C[C@H]4N(C)C3)(C(C)C)C(=O)N12.CS(=O)(=O)O
bromocriptine
CC(C)C[C@H]1C(=O)N2CCC[C@H]2[C@]2(O)O[C@](NC(=O)[C@@H]3C=C4c5cccc6[nH]c(Br)c(c56)C[C@H]4N(C)C3)(C(C)C)C(=O)N12.CS(=O)(=O)O
bromocriptine mesylate

Reagents

None

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Otherfitted with a USP induction port (<USP 601> Pharmacopeial Previews 22, 3065 (1995))
  2. 2
    Filtrationfilter
  3. 3
    Otherwere actuated per test, with an interval of at least 30 seconds between shots
  4. 4
    Temperatureto prevent cooling of the can
  5. 5
    Otherresultant moisture condensation
  6. 6
    Filtrationfilter (corresponding to particles of MMAD less than 3.3 μm)

Procedure

The formulations were tested on an Andersen™ cascade impactor to determine their aerodynamic particle properties. The cascade impactor was operated at 28.3 I/min and fitted with a USP induction port (<USP 601> Pharmacopeial Previews 22, 3065 (1995)). The particle size distributions were fractionated into mass of drug deposited on the pMDI actuator, USP induction port, eight stages and terminal filter. Five shots were actuated per test, with an interval of at least 30 seconds between shots to prevent cooling of the can and resultant moisture condensation. The bromocriptine content in each sample was determined by HPLC. The percentage of the total dose deposited from stage 4 to the terminal filter (corresponding to particles of MMAD less than 3.3 μm) was considered to be the fine particle fraction.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07582284B2uspto-grants-2009_09