Reference

Determination of itopride in human plasma by liquid chromatography coupled to tandem mass spectrometric detection: Application to a bioequivalence study

All Rights Reserved. Determination of itopride in human plasma by liquid chromatography coupled to tandem mass spectrometric detection: Application to a bioequivalence study. Lee, Heon-Woo; Seo, Ji-Hyung; Choi, Seung-Ki; Lee, Kyung-Tae ( College of Pharmacy, Kyung Hee University, Seoul 130-701, S. Korea). Analytica Chimica Acta, 583(1), 118-123 (English) 2007 Elsevier B.V. CODEN: ACACAM. ISSN: 0003-2670. DOCUMENT TYPE: Journal CA Section: 1 (Pharmacology) A simple method using a one-step liq.-liq. extn. (LLE) with Bu acetate followed by high-performance liq. chromatog. (HPLC) with pos. ion electrospray ionization tandem mass spectrometric (ESI-MS/MS) detection was developed for the detn. of itopride in human plasma, using sulpiride as an internal std. (IS). Acquisition was performed in multiple reaction monitoring (MRM) mode, by monitoring the transitions: m/z 359.5 > 166.1 for itopride and m/z 342.3 > 111.6 for IS, resp. Analytes were chromatographed on an YMC C18 reverse-phase chromatog. column by isocratic elution with 1 mM ammonium acetate buffer-methanol (20: 80, vol./vol.; pH 4.0 adjusted with acetic acid). Results were linear (r 2 = 0.9999) over the studied range (0.5-1000 ng mL-1) with a total anal. time per run of 2 min for LC-MS/MS. The developed method was validated and successfully applied to bioequivalence studies of itopride hydrochloride in healthy male volunteers.Except for chemicals metioned above, 122892-31-3 is also used. .

Method for preparing 4-[2-(dimethylamino)ethoxy]benzylamine as itopride hydrocloride salt intermediate

Method for preparing 4-[2-(dimethylamino)ethoxy]benzylamine as itopride hydrocloride salt intermediate. Kim, Dong Yeon; Kim, Jae Gun; Cho, Dae Jin; Lee, Gong Yeal; Kim, Hong Youb; Woo, Seok Hun (Il Yang Pharm. Co., Ltd, S. 122892-31-3 are also occured in this study. 122892-31-3 is just another one chemical used in this study. Korea). PCT Int. Appl. WO 2006011696 A1 2 Feb 2006, 16 pp. DESIGNATED STATES: W: AE, AG, AL, AM, AT, AU, AZ, BA, BB, BG, BR, BW, BY, BZ, CA, CH, CN, CO, CR, CU, CZ, DE, DK, DM, DZ, EC, EE, EG, ES, FI, GB, GD, GE, GH, GM, HR, HU, ID, IL, IN, IS, JP, KE, KG, KP, KZ, LC, LK, LR, LS, LT, LU, LV, MA, MD, MG, MK, MN, MW, MX, MZ, NA, NI, NO, NZ, OM, PG, PH, PL, PT, RO, RU, SC, SD, SE, SG, SK, SL, SY, TJ, TM, TN, TR, TT, TZ, UA, UG, US, UZ, VC, VN, YU, ZA, ZM, ZW; RW: AT, BE, BF, BJ, CF, CG, CH, CI, CM, CY, DE, DK, ES, FI, FR, GA, GB, GR, IE, IT, LU, MC, ML, MR, NE, NL, PT, SE, SN, TD, TG, TR. (English). (World Intellectual Property Organization). CODEN: PIXXD2. CLASS: ICM: C07C213-06. APPLICATION: WO 2004-KR2342 15 Sep 2004. PRIORITY: KR 2004-58972 28 Jul 2004. DOCUMENT TYPE: Patent CA Section: 25 (Benzene, Its Derivatives, and Condensed Benzenoid Compounds) The present invention relates to a novel method for prepg. an itopride×hydrochloride mediate, which is useful as a digestive tract activator. More particularly, the present invention provides a method for prepg. 4-[2-(dimethylamino)ethoxy]benzylamine (I) in high yield and using a method that lowers the cost, uses a selective reaction, and is safe to humans and the environment. Thus, dropwise addn. of NaH to 2-(dimethylamino)ethanol at 0°C followed by raising the temp. to 130-140°C and adding 4-fluorobenzylamine gave I in 91% yield. Alternately, I could be prepd. by reacting 4-hydroxybenzonitrile with KOH in acetone followed by slow addn. of 2-(dimethylamino)ethyl chloride giving 4-[(2-dimethylamino)ethoxy]benzonitrile which was then reduced to I in 80% yield. ..