CRYSTALLINE FORM OF TERT-BUTYL [(S)-4-METHYL-1-((R)-2-METHYLOXIRAN-2-YL)-1-OXOPENTAN-2-YL] CARBAMATE AND PROCESS FOR ITS PREPARATION
Publication Date: 2014-Feb-27
The IP.com Prior Art Database
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CRYSTALLINE FORM OF TERT-BUTYL [(S)-4-METHYL-1-((R)-2- METHYLOXIRAN-2-YL)-1-OXOPENTAN-2-YL] CARBAMATE AND PROCESS FOR ITS PREPARATION
Tert-butyl [(S)-4-methyl-1-((R)-2-methyloxiran-2-yl)-1-oxopentan-2-yl] carbamate, referred as to 'Compound Boc-PAMO', of the following formula:
is an intermediate in the synthesis of (S)-4-Methyl-N-((S)-1-(((S)-4-methyl-1-((R)-2-methyloxiran- 2-yl)-1-oxopentan-2-yl)amino)-1-oxo-3-phenylpropan-2-yl)-2-((S)-2-(2-morpholinoacetamido)-4- phenylbutanamido) pentanamide.
Provided herein after, is a crystalline form of tert-butyl [(S)-4-methyl-1-((R)-2- methyloxiran-2-yl)-1-oxopentan-2-yl] carbamate and a process for its preparation.
Crystalline Form of Compound Boc-PAMO
The crystalline form of Compound Boc-PAMO can be characterized by an X-ray powder diffraction pattern having peaks at 6.4, 8.5, 12.5, 17.0, 17.6, 18.0, 18.9, 19.9, 21.7, 23.7, 25.2 and
27.2 degrees two theta ± 0.2 degrees two theta; and/or an X-ray powder diffraction pattern as depicted in Figure 1.
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Experimental: XRPD method
Samples after being powdered in a mortar and pestle are applied directly on silicon plate holder. The X-ray powder diffraction pattern was measured with Philips X'Pert PRO X-ray powder diffractometer, equipped with Cu irradiation source =1.54184 Ǻ (Ǻngström), X'Celerator (2.022º 2 Ө) detector. Scanning parameters: angle range: 3-40 deg., step size 0.016...