Certificate Of Analysis

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1 Certificate f Analysis Compound: -Hydroxy Propranolol Molecular Formula: C H N. (mw base =.) Structure: MW =. base H 8 0 H C H N -Hydroxy Propranolol "FR CHEMICAL USE NLY" Synonyms: (CA index name) -[(-Methylethyl)amino]--(-{-hydroxy}-naphthalenyloxy)--Propanol Summary of Analytical Results:. H NMR proton data (DMS-d ): The results of H NMR spectroscopic analysis are consistent with the structure of -[(-Methylethyl)amino]--(-{-hydroxy}-naphthalenyloxy)--propanol. The aromatic region (8.-. ppm) of the H-NMR exhibits numerous proton resonances. These aromatic protons are consistent with a disubstituted naphthalenyl aromatic ring. Integration and proton-proton coupling reveals two separate spin systems; an ABX and an ABC. Aliphatic proton resonances are exhibited between. ppm and ppm. These resonances reveal protons separated into two isolated contiguously coupled spin systems. ne spin system is an isopropyl and the second is a,,-tri-substituted propyl spin system. All features are consistent with the structure of -Hydroxy Propranolol.. H NMR -D gcsy data (DMS-d ): The data developed from the -D CSY experiment reveal spin-spin -bond (vicinal) coupling via off axis contour correlations. The illustrated -D gcsy is consistent with an isopropyl spin system, a,,-tri-substituted propyl spin system, an aromatic ABX and an ABC spin system. Atlantic Analytical Laboratory: Certificate of Analysis Spectra and Structure //00 Page of

2 . H NMR -D GCSY data (DMS-d ): The data developed from the -D GCSY experiment (eq. TCSY exp) reveal isolated contiguously coupled spin systems. The illustrated portions of the -D GCSY s are consistent with an isopropyl spin system, an aromatic ABX and an ABC spin system. The -D gcsy and -D GCSY data are summarized.... H NMR -D ne difference experimental data (DMS-d ): The results of H NMR -D ne difference spectroscopic analysis are consistent with the structure of -[(-Methylethyl)amino]-- (-{-hydroxy}-naphthalenyloxy)--propanol. These data reveal through space or proximal located spins. These data are based upon relaxation phenomenon. Thus, pre-irradiation of an isolated resonance reveals, via a difference spectrum, proximal protons. C NMR data (DMS- d ): The data developed from the -D APT Carbon experiment modulate the carbon data based upon the one bond proton-carbon coupling (JHC Hz). The data is expressed via up and down peak depending upon the magnitude of their one bond coupling. The data are consistent with the structure of -Hydroxy Propranolol H - C NMR -D ghsqc data (DMS-d ): The data developed from the -D ghsqc experiment reveal one bond cross correlations between protons and carbons in a two dimensional format. Assignments in either domain allow direct assignment of the opposite domain from their cross contours. The assignments are based upon data and conclusions obtained from earlier experiments, i.e. -D gcsy, -D ne difference data, -D APT carbon data, chemical shifts and coupling constant considerations. The data are consistent with the structure of - Hydroxy Propranolol. H - C NMR -D HMBC data (DMS-d ): The data developed from the -D HMBC experiment reveal -bond cross correlations between protons and carbons in a two dimensional format. The experiment is optimized with a time delay for 8 Hz coupling ( J HC coupling). ccasionally a - bond correlation will appear. Furthermore, the suppression on -bond couplings also appears in the spectra due to non-optimal bird-pulse suppression. Important -bond correlations are summarized in this structural illustration: 8. IR (HCl salt in a KBr pellet): The Infrared data are consistent with the structure of -Hydroxy Propranolol. The strongest absorbance is exhibited in the broad band between cm -. This is consistent with hydroxyl moiety in the molecule. Asymmetric deformation modes of stretching for the naphthenyl ring occur as bands between 8 and 00 cm -, symmetric modes occur between 0 and 00 cm -. Aromatic character is also expressed in the area between 8 - cm -, the result of out-of-plane proton-carbon bending. Aliphatic character (, 80 and 8 cm - ) is revealed in numerous areas of the spectrum and the strong bands at 0 and cm - are consistent with oxygen-carbon stretching.. LC/UV/ESI/MS: The sample was evaluated by HPLC/UV/ElectroSpray Ionization/MS. The results are consistent with the structure of -Hydroxy Propranolol. The molecular ion (M+H) + is observed at Daltons along with structurally related fragment ions. No unrelated ions were observed by mass spectrometry under the UV peak. The % Total Area of -Hydroxy Propranolol calculated at 0 nm is %. 0. TLC Analysis: via Thin Layer Chromatography via Analtech Uniplate - Silica Gel GHLF shows one spot (R.F. = 0.; in methylene chloride : methanol : ammonia [0:0:] and R.F. = 0.; in ethyl acetate : methanol : ammonia [80 : 0 : ]. Atlantic Analytical Laboratory: Certificate of Analysis Spectra and Structure //00 Page of

3 Fig. H-NMR of Propranolol, structure and spectra ' H H 0 ' -Hydroxy Propanolol H NMR at 00 MHz in DMS-D 8 DMS Atlantic Analytical Laboratory: Certificate of Analysis Spectra and Structure //00 Page of

4 Fig. H NMR -D gcsy data (DMS-d ), structure and spectra H H 0 8,, Atlantic Analytical Laboratory: Certificate of Analysis Spectra and Structure //00 Page of

5 Fig. H NMR -D GCSY data (DMS-d ), structure and spectra H H 0 -D GCSY ' Atlantic Analytical Laboratory: Certificate of Analysis Spectra and Structure //00 Page of

6 Fig B. -D gcsy and -D gcsy data are summarized -D gcsy vicinally coupled spin systems -D GCSY isolated contiguously coupled spin systems H 8 0 H H 8 0 H Atlantic Analytical Laboratory: Certificate of Analysis Spectra and Structure //00 Page of

7 Fig. H -NMR -D ne, structure and spectra H H 0 Atlantic Analytical Laboratory: Certificate of Analysis Spectra and Structure //00 Page of

8 Fig. C NMR of -Hydroxy Propranolol, structure and spectra H H 0 8 DMS 0 APT (GASPE) J-modulated C data H 8 0 H x-ch x-ch (aromatic) x-ch x-c (Quat.) x-ch (alphatic) Atlantic Analytical Laboratory: Certificate of Analysis Spectra and Structure //00 Page 8 of

9 Fig. H - C NMR -D ghsqc data (DMS-d ), structure and spectra H H 0 ghsqc one bond correlations 8 8 Atlantic Analytical Laboratory: Certificate of Analysis Spectra and Structure //00 Page of

10 Fig. H - C NMR -D HMBC data (DMS-d ), structure and spectra H H 0 ghmbc and bond correlations 8,,,,, 8, Atlantic Analytical Laboratory: Certificate of Analysis Spectra and Structure //00 Page 0 of

11 Fig B. Important -bond correlations are summarized in this structural illustration: -D HMBC experimental data selected important correlations -bond corr. H 8 0 H Atlantic Analytical Laboratory: Certificate of Analysis Spectra and Structure //00 Page of

12 Fig 8. IR (HCl salt in a KBr pellet) A cm- Atlantic Analytical Laboratory: Certificate of Analysis Spectra and Structure //00 Page of

13 Fig. LC/UV/ESI/MS LC -ESI+ [M + H]+ MW = LC / MS with ESI+ mode PDA TIC LC / ESI + [M + H]+ MW = Atlantic Analytical Laboratory: Certificate of Analysis Spectra and Structure //00 Page of

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