US 11,719,488 B2
Lyophilization process and a teverelix-TFA lyophilizate obtained thereby
Guy Poland, Bristol (GB); and Francois Boutignon, Clermont-Ferrand (FR)
Assigned to Antev Limited, London (GB)
Appl. No. 17/255,372
Filed by Antev Limited, London (GB)
PCT Filed Jul. 2, 2019, PCT No. PCT/EP2019/067733
§ 371(c)(1), (2) Date Dec. 22, 2020,
PCT Pub. No. WO2020/007860, PCT Pub. Date Jan. 9, 2020.
Claims priority of application No. 18181960 (EP), filed on Jul. 5, 2018.
Prior Publication US 2021/0239397 A1, Aug. 5, 2021
Int. Cl. A61K 39/395 (2006.01); F26B 5/06 (2006.01); A61K 9/19 (2006.01); A61K 38/09 (2006.01); A61K 47/12 (2006.01)
CPC F26B 5/06 (2013.01) [A61K 9/19 (2013.01); A61K 38/09 (2013.01); A61K 47/12 (2013.01)] 13 Claims
 
1. A lyophilization process for preparing a teverelix-TFA lyophilizate,
said process comprises the following steps:
a) providing a lyophilization suspension by mixing teverelix and trifluoroacetate at a molar ratio of teverelix to trifluoroacetate sufficient for providing a microcrystalline teverelix-TFA suspension without formation of a gel, and wherein the suspension comprises at least 2.1 mol trifluoroacetate per mol teverelix,
b) lyophilizating the lyophilization suspension from the step a) thereby providing a teverelix-TFA lyophilizate having a mol content of trifluoroacetate per mol teverelix which is lower than the mol content of trifluoroacetate per mol teverelix in the lyophilization suspension, wherein the step a) further comprises the following steps:
a′) centrifuging or filtering the microcrystalline teverelix-TFA suspension thereby respectively providing a teverelix-TFA pellet or a teverelix-TFA filter cake with a a molar ratio of teverelix to TFA of 1:1.70 to 1:1.85, wherein the teverelix in the teverelix-TFA pellet or teverelix-TFA filter cake is microcrystalline, and
a″) suspending said teverelix-TFA pellet or said teverelix-TFA filter cake in an aqueous suspension solution.