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PURE (1S,3S,7S,10R,11S, 12S, 16R)-7,11-DIHYDROXY-8,8,10,12,16- PENTAMETHYL-3-[(E)-1-METHYL-2-(2-METHYLTHIAZOL-4-YL)VINYL]-17- OXA-4-AZABICYCLO[14.1.0]HEPTADECANE-5,9-DIONE

IP.com Disclosure Number: IPCOM000201014D
Publication Date: 2010-Nov-04
Document File: 2 page(s) / 50K

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The IP.com Prior Art Database

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    PURE (1S,3S,7S,10R,11S, 12S, 16R)-7,11-DIHYDROXY-8,8,10,12,16- PENTAMETHYL-3-[(E)-1-METHYL-2-(2-METHYLTHIAZOL-4-YL)VINYL]-17- OXA-4-AZABICYCLO[14.1.0]HEPTADECANE-5,9-DIONE

    (1S,3S,7S,10R,11S, 12S, 16R)-7,11-Dihydroxy-8,8,10,12,16-pentamethyl-3-[(E)-1- methyl-2-(2-methylthiazol-4-yl)vinyl]-17-oxa-4-azabicyclo[14.1.0]heptadecane-5,9-dione (referred to as IXB) has the following formula:

O

O O

O

    Described herein below a process for preparing pure IXB, in a crystalline form. Preparation of pure IXB

    IXB (crude, 1 g) was dissolved in acetone (10 mL) at room temperature and a solution was formed. The solution was heated to reflux (about 56°C) for 1 h and then it was cooled down to room temperature over 1 h. The cooled mixture was stirred for 1 h and then it was filtered. The collected solid was washed with acetone (2 mL) and dried at 40°C under vacuum. Yield 50%; HPLC purity: 99.94%. The sample was analyzed by PXRD.

N

S

OH

HN

H

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XRD method

    X-ray powder diffraction (XRD) was performed on Philips X'Pert PRO powder diffractometer equipped with X'Celerator detector (active length 2 = 2.022°), CuK radiation, = 1.54184 Å at laboratory temperature 22-25°C.

Prior to analysis the samples were gently ground by means of mortar and pestle in order to obtain a fine powder and applied directly on silicon zero background holder.The scanning parameters were: range: 3-40 degrees two-theta; scan mode: continuous sca...