LFA-1 inhibitor and methods of preparation and polymorph thereof
Methods of preparation and purification of a compound of Formula I, intermediates thereof, a polymorph thereof, and related compounds are disclosed. Formulations and uses thereof in the treatment of LFA-1 mediated diseases are also disclosed.
1. A method of purifying a compound of Formula I:
or a salt thereof, comprising the steps:
a) obtaining crude compound of Formula I or a salt thereof and recrystallizing said crude compound with aqueous acetone; and
b) isolating said compound of Formula I or a salt thereof by removal of aqueous acetone.
2. The method of claim 1 , wherein said aqueous acetone is used in an amount of about 7 volumes.
3. The method of claim 1 , wherein said aqueous acetone is about 30% aqueous acetone.
4. The method of claim 1 , further comprising addition of a pH modifier to produce a pH of less than about 5.
5. The method of claim 4 , wherein said method produces a pH between about 1 and about 5.
6. The method of claim 4 , wherein said pH modifier is selected from an organic or mineral acid.
7. The method of claim 4 , wherein said pH modifier is hydrochloric acid.
8. The method of claim 1 , wherein said removal of aqueous acetone is by filtration.
9. The method of claim 1 , wherein said method is performed for a period of time ranging from about 1 hour to about 48 hours.