Granted Patent B2

US 12,358,861 · App. 18/386,906 · Granted Jul 15, 2025

Inventors: Timothy James Morley (Harrogate, GB); Ronnie Maxwell Lawrence (Upper Gravenhurst, GB); Naseem Amin (London, GB)

Assignee: ORPHALAN S.A.

C07C211/14C07C209/84A61K9/0053C07B2200/13

Abstract

Claims (15)

1. A crystalline form of triethylenetetramine tetrahydrochloride Form B having at least one of the following characteristics:

(i) an XRPD pattern having at least two peaks selected from the peaks at 22.9, 25.4, 25.8, 26.6, 34.6 and 35.3±0.1° 2θ; and

(ii) a Raman spectrum having at least two peaks selected from the peaks at a Raman shift of 943, 1173, 1527 and 1612±5 cm −1 ,

and which contains no more than 10 wt % of triethylenetetramine tetrahydrochloride Form A having an XRPD pattern having peaks at 25.2 and 35.7±0.1° 2θ, wherein XRPD pattern peaks are as measured using a wavelength of 1.5418 Å,

and wherein the crystalline form is obtainable by a method comprising:

adding an anti-solvent to an aqueous solution of triethylenetetramine tetrahydrochloride and collecting the crystals obtained, wherein the anti-solvent addition is carried out at a temperature of about 15° C. or below.

2. A crystalline form of triethylenetetramine tetrahydrochloride which consists essentially of triethylenetetramine tetrahydrochloride Form B having at least one of the following characteristics:

(i) an XRPD pattern having at least two peaks selected from the peaks at 22.9, 25.4, 25.8, 26.6, 34.6 and 35.3±0.1° 2θ; and

(ii) a Raman spectrum having at least two peaks selected from the peaks at a Raman shift of 943, 1173, 1527 and 1612±5 cm −1

wherein XRPD pattern peaks are as measured using a wavelength of 1.5418 Å.

3. A method of reducing copper levels in a subject, which method comprises the administration to said subject of an effective amount of a crystalline form of triethylenetetramine tetrahydrochloride Form B having at least one of the following characteristics:

(i) an XRPD pattern having at least two peaks selected from the peaks at 22.9, 25.4, 25.8, 26.6, 34.6 and 35.3±0.1° 2θ; and

(ii) a Raman spectrum having at least two peaks selected from the peaks at a Raman shift of 943, 1173, 1527 and 1612±5 cm −1 ;

and which contains no more than 10 wt % of triethylenetetramine tetrahydrochloride Form A having an XRPD pattern having peaks at 25.2 and 35.7±0.1° 2θ,

wherein XRPD pattern peaks are as measured using a wavelength of 1.5418 Å.

Assignments (3)

Priority Claims (1)

Continuity (5)

References Cited (26)