IP Library Granted Patent US 11,395,809
Granted Patent B2
US 11,395,809 · App. 16/943,558 · Granted Jul 26, 2022

Crystalline polymorphic forms of monosodium n-[-8-(2-hydroxybenzoyl)amino]caprylate

Inventors: Halina Levchik (Croton On Hudson, NY); Shingai Majuru (Brewster, NY); Brahma Singh (Jamaica, NY); Jamila Harris (Flushing, NY)
Assignee: NOVO NORDISK NORTH AMERICA OPERATIONS A/S
A61K31/197A61J3/02A61K9/2095A61K31/198A61K45/06C07C235/60A61K2300/00
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Quick Facts
Patent No.
US 11,395,809
App. No.
16/943,558
Granted
Jul 26, 2022
Kind
B2
Abstract

The present invention relates to crystalline polymorphic forms of monosodium N-[8-(2-hydroxybenzoyl)amino] caprylate (“SNAC”), including two hydrates, a methanol solvate, and an ethanol solvate, of SNAC. More specifically, the present invention provide six polymorphic forms of SNAC (hereafter referred to as Forms I-V). The present invention also provides an amorphous form of SNAC.

Claims (8)

1. A crystalline anhydrous monosodium N-[8-(2-hydroxybenzoyl)amino]caprylate exhibiting an X-ray powder diffraction pattern having a peak at 17.04±0.2° 2Θ, 23.28±0.2° 2Θ, or both.

2. The crystalline anhydrous monosodium N-[8-(2-hydroxybenzoyl)amino]caprylate of claim 1 , wherein the crystalline anhydrous monosodium N-[8-(2-hydroxybenzoyl)amino]caprylate exhibits X-ray powder diffraction pattern peaks at 17.04 and 23.28±0.2° 2Θ.

3. The crystalline anhydrous monosodium N-[8-(2-hydroxybenzoyl)amino]caprylate of claim 1 , wherein the crystalline anhydrous monosodium N-[8-(2-hydroxybenzoyl)amino]caprylate is prepared by a process comprising heating Form I, II, III, V, or VI of monosodium N-[8-(2-hydroxybenzoyl)amino]caprylate or a mixture thereof to a temperature between about 110° C. and the melting point of monosodium N-[8-(2-hydroxybenzoyl)amino]caprylate for a sufficient time to yield Form IV.

4. The crystalline anhydrous monosodium N-[8-(2-hydroxybenzoyl)amino]caprylate of claim 3 , wherein the Form II of monosodium N-[8-(2-hydroxybenzoyl)amino]caprylate is heated to between about 150° C. and the melting point of monosodium N-[8-(2-hydroxybenzoyl)amino]caprylate for a sufficient time to yield Form IV.

5. A crystalline anhydrous monosodium N-[8-(2-hydroxybenzoyl)amino]caprylate exhibiting an X-ray powder diffraction pattern having a melting point of 199° C.

6. The crystalline anhydrous monosodium N-[8-(2-hydroxybenzoyl)amino]caprylate of claim 5 , wherein the crystalline anhydrous monosodium N-[8-(2-hydroxybenzoyl)amino]caprylate is prepared by a process comprising heating Form I, II, III, V, or VI of monosodium N-[8-(2-hydroxybenzoyl)amino]caprylate or a mixture thereof to a temperature between about 110° C. and the melting point of monosodium N-[8-(2-hydroxybenzoyl)amino]caprylate for a sufficient time to yield Form IV.

7. The crystalline anhydrous monosodium N-[8-(2-hydroxybenzoyl)amino]caprylate of claim 6 , wherein the Form II of monosodium N-[8-(2-hydroxybenzoyl)amino]caprylate is heated to between about 150° C. and the melting point of monosodium N-[8-(2-hydroxybenzoyl)amino]caprylate for a sufficient time to yield Form IV.

8. The crystalline anhydrous monosodium N-[8-(2-hydroxybenzoyl)amino]caprylate of claim 1 , wherein the crystalline anhydrous monosodium N-[8-(2-hydroxybenzoyl)amino]caprylate exhibits X-ray powder diffraction pattern peaks at 8.61, 17.04, and 23.28±0.2°2Θ.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 22, 2021
From: EMISPHERE TECHNOLOGIES, INC.
To: NOVO NORDISK NORTH AMERICA OPERATIONS A/S
Reel/Frame 056750/0169 →
Continuity (8)
Continuation 16212428 · Dec 6, 2018
Continuation 15668236 · Aug 3, 2017
Continuation 15049313 · Feb 22, 2016
Continuation 14138787 · Dec 23, 2013
Continuation 11568753
Provisional Application 60619418 · Oct 15, 2004
Provisional Application 60569476 · May 6, 2004
Related Publication 20210177792A1 · Jun 17, 2021