Browse Prior Art Database

5-[2-[4-(1,2-benzisothiazol-3-yl)-1-piperazinyl]ethyl]-6-chloro-1,3-dihydro-2 H -indol-2-one, monohydrochloride intermediates-(BITP-HCl; CEI) Crystal forms

IP.com Disclosure Number: IPCOM000018792D
Publication Date: 2003-Aug-10
Document File: 4 page(s) / 153K

Publishing Venue

The IP.com Prior Art Database

This text was extracted from a PDF file.
At least one non-text object (such as an image or picture) has been suppressed.
This is the abbreviated version, containing approximately 73% of the total text.

Page 1 of 4

5-[2-[4-(1,2-benzisothiazol-3-yl)-1-piperazinyl]ethyl]-6-chloro-1,3- dihydro-2 H -indol-2-one, monohydrochloride intermediates- (BITP·HCl; CEI) Crystal forms

N.HCl

N H

N

N

S

BITP.HCl

Cl

O

Cl

CEI

N-(1,2-benzisothiazol-3-yl) piperazine (BITP) and 5-(2-chloroethyl)-oxindole (CEI) are used as intermediate in the preparation of 5-[2-[4-(1,2-benzisothiazol-3-yl)-1- piperazinyl]ethyl]-6-chloro-1,3-dihydro-2 H -indol-2-one, monohydrochloride. Samples of BITP·HCl, CEI were analyzed by X-Ray Powder diffraction and found to contain different crystal forms (α, β, β-1). Table I summarizes the various samples and suppliers.

XRD diffractograms of BITP·HCl (α) and CEI (β, β-1) are shown in fig. 1-3. Main XRD peaks for the various forms: α, β, β-1 are listed in Table II. X-Ray Powder Diffractions were performed on ARL (Scintag) X-Ray powder diffractometer

model X'TRA, Cu-tube, solid state detector. A round standard aluminum sample holder with round zero background quartz plate was used. Scanning parameters: range 2-40 deg.2Θ, continuous scan, rate 3 deg/min.

[This page contains 2 pictures or other non-text objects]

Page 2 of 4

Table I

Table II

Sample No. Supplier crystal form

BITP.HCl - 1 Xiamen MCHEM Industry CO., LTD α BITP.HCl - 2 Yancheng lyve chem. α BITP.HCl - 3 Topharman α

CEI - 1 Xiamen MCHEM Industry CO., LTD β CEI - 2 Yancheng lyve chem. β-1

Crystal form XRD peaks (2θ)

α 7.9, 12.9, 14.1, 15.7, 17.1, 18.8, 19.9, 20.7, 23.1, 23.7, 24.0, 25.2,

26.8, 27....