Browse Prior Art Database

Process of preparation of Crystal III of 5-Chloro-6-[(2-imino-1-pyrrolidinyl)methyl]-2,4(1H,3H)-pyrimidinedione hydrochloride having low content of residual solvent

IP.com Disclosure Number: IPCOM000250259D
Publication Date: 2017-Jun-20
Document File: 3 page(s) / 234K

Publishing Venue

The IP.com Prior Art Database

This text was extracted from a PDF file.
This is the abbreviated version, containing approximately 71% of the total text.

Process of preparation of Crystal III of 5-Chloro-6-[(2-imino-1-pyrrolidinyl)methyl]-

2,4(1H,3H)-pyrimidinedione hydrochloride having low content of residual solvent

5-Chloro-6-[(2-imino-1-pyrrolidinyl)methyl]-2,4(1H,3H)-pyrimidinedione hydrochloride has the

following chemical structure (referred to herein as Compound I):

Provided are processes for preparing crystal III of compound I having low content of residual

solvent.

Powder X-ray Diffraction (XRPD) method

X-ray diffraction was performed on X-Ray powder diffractometer:

PANalytical X’Pert Pro; CuKα radiation (λ = 1.54 Å); PIXcel 1D detector; Back-loading Sample

Holder. Prior to analysis, the sample was adjusted into a cavity of the sample holder ring and the

surface of the sample was smoothed by means of a press block and holder ring was locked in

holder base.

Measurement parameters:

Scan range: 3 – 50 degrees 2-theta;

Scan mode: continuous;

Step size: 0.0065652 degrees;

Time per step: 20.4 s;

Sample spin: 1 s;

Sample holder: Back-loading Sample Holder.

Example

Example 1: Preparation of crystal III of 5-Chloro-6-[(2-imino-1-pyrrolidinyl)methyl]-

2,4(1H,3H)-pyrimidinedione Hydrochloride.

To the cooled mixture of 5-Chloro-6-[(2-imino-1-pyrrolidinyl)methyl]-2,4(1H,3H)-

pyrimidinedione 1 (25g), in methanol2

(150ml), slowly added hydrochloric acid (6N; 38ml) and

resulting reaction mixture was stirred for 30 to 60 minutes at 5-10 0 C. Product was isolated by

filtration and washed with methanol. After drying 27.2g (94.6%) dry p...