1,2-Bis(2-aminophenoxy)ethyl-N,N,N',N'-acetic acid methyl ester

http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0103-50532014000100014&lng=en&nrm=iso&tlng=en

1,2-Bis(2-aminophenoxy)ethyl-N,N,N',N'-acetic acid methyl ester 4

Compound 3 (2.44 g, 0.01 mol) was dissolved in MeCN (10 mL), then (i-Pr)₂NEt (6 mL) and methyl bromoacetate (3 mL) were added to the mixture with stirring. The reaction mixture was refluxed for 24 h. After the reaction, the mixture was cooled down, poured into EtOAc (20 mL), and filtered to remove the generated white solid. The combined EtOAc filtrates were concentrated in vacuo to give an oily solid, then adding a little methanol, white solid was generated, filtered, air dried and recrystallized in MeOH to give white solid 4. Yield 87%; 

m.p. 94-95 ºC;  

¹H NMR (CDCl₃, 400 MHz) δ 6.85 (m, 8H), 4.27 (s, 4H), 4.15 (s, 8H), 3.56 (s, 12H); 

IRν/cm^-1 3067, 2993, 2951, 2921, 2888, 1748, 1596, 1509, 1173, 742, 706.

Journal of the Brazilian Chemical Society

Print version ISSN 0103-5053

J. Braz. Chem. Soc. vol.25 no.1 São Paulo Jan. 2014

http://dx.doi.org/10.5935/0103-5053.20130276 

ARTICLE

Structural study and fluorescent property of a novel organic microporous crystalline material

Zhao Cheng; Bingqin Yang^*; Meipan Yang; Binglin Zhang

Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, 710069 Xi'an, China

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N,N-Dimethyl-5-nitropyridin-2-amine

N,N-Dimethyl-5-nitropyridin-2-amine³⁰ (3d)

Yellow solid; mp 155-157 °C; 

¹H NMR (DMSO-d₆, 400 MHz) 

δ 9.02 (d, 1H, J 2.8 Hz), 

8.26 (dd, 1H, J 9.2; 2.8 Hz), 

6.80 (d, 1H, J 9.2 Hz), 

3.25 (s, 6H); 

IR (KBr) ν_max/cm^-1: 2924, 2854, 1597, 1335, 1295, 1118, 810; 

MS (CI method): 168 (M+1, 100%).

30. Heindel, N. D.; Kannewell, P. D.; Chem. Commun. 1969, 38.         [ Links ]

N,N-bis(5-methyl-2 hydroxybenzyl)methylamine (MMD)

1H NMR

Figure 6. ¹H-¹H NOESY spectra of (a) MMD; (b) Ce(III)-MMD complex in CDCl₃. - See more at: http://www.mdpi.com/1422-0067/12/7/4365/htm#sthash.ExEZ0GaQ.dpuf

NOESY..........http://www.mdpi.com/1422-0067/12/7/4365/htm











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Figure 6. ¹H-¹H NOESY spectra of (a) MMD; (b) Ce(III)-MMD complex in CDCl₃. - See more at: http://www.mdpi.com/1422-0067/12/7/4365/htm#sthash.ExEZ0GaQ.dpuf

Figure 6. ¹H-¹H NOESY spectra of (a) MMD; (b) Ce(III)-MMD complex in CDCl₃. - See more at: http://www.mdpi.com/1422-0067/12/7/4365/htm#sthash.ExEZ0GaQ.dpuf

Figure 6. ¹H-¹H NOESY spectra of (a) MMD; (b) Ce(III)-MMD complex in CDCl₃. - See more at: http://www.mdpi.com/1422-0067/12/7/4365/htm#sthash.ExEZ0GaQ.dpuf

N,N-Dimethyl-5-nitropyridin-2-amine

N,N-Dimethyl-5-nitropyridin-2-amine³⁰ (3d)

Yellow solid; mp 155-157 °C; ¹H NMR (DMSO-d₆, 400 MHz) δ 9.02 (d, 1H, J 2.8 Hz), 8.26 (dd, 1H, J 9.2; 2.8 Hz), 6.80 (d, 1H, J 9.2 Hz), 3.25 (s, 6H); IR (KBr) ν_max/cm^-1: 2924, 2854, 1597, 1335, 1295, 1118, 810; MS (CI method): 168 (M+1, 100%).

30. Heindel, N. D.; Kannewell, P. D.; Chem. Commun. 1969, 38. 

Journal of the Brazilian Chemical Society

Print version ISSN 0103-5053

J. Braz. Chem. Soc. vol.21 no.8 São Paulo  2010

http://dx.doi.org/10.1590/S0103-50532010000800005

see

http://www.scielo.br/scielo.php?pid=S0103-50532010000800005&script=sci_arttext

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N,N-Dimethyltryptamine

DMT Mass Spectra

DMT Mass Spectra

DMT Mass Spectra (expanded)

DMT Mass Spectra (Expanded)

Quantification

• • Blood:
• GC Column: DB-1 fused silica capillary (30 m  0.32 mm i.d., 0.2 mm). Carrier gas: H2, 3 or 3.5 mL/min. Temperature: 230° and 280° . SID. Limit of

detection, 0.5 mg/L [Ishii et al. 1997].

• GC-MS Column: SE-30 (18 m  0.33 mm i.d.). Carrier gas: He, 2 mL/min. Temperature: 200° . EI ionisation at 70 eV, SIM acquisition mode. Limit of detection, 10 ng/L [Walker et al. 1979].
• Plasma GC Column: 5% phenyl methyl silicone capillary (12 m  0.2 mm i.d.,0.33 mm). Carrier gas: H2, 0.7 mL/min. Temperature programme: 70° for 1 min to 120° at 30° /min to 280° at 20° /min. Limit of quantification, 1.6 mg/L [Yritia et al. 2002].
• HPLC Column: Supelcosil LC-DB-8 (150 Â 4.6 mm i.d., 5 mm). Mobile phase: methanol : acetonitrile : 0.1 mol/L ammonium acetate (pH 6.9, 20 : 20 : 60), flow rate 2.0 mL/min. Fluorescence detection (lex1⁄4 232 nm, lem1⁄4 351 nm or lex1⁄4 340nm, lem1⁄4 495 nm). Limit of quantification, 2 mg/L [Callaway et al. 1996].

• • Urine
• GC See Blood [Ishii et al. 1997].
• GC-MS Column: 1% OV-101 on 80/100 mesh Gas-Chrom Q. Temperature:190° . EI ionisation, MID. Limit of detection, 100 ng/L [Raisanen, Karkkainen 1979].
• LC-MS EI ionisation at 70 eV. SRM acquisition mode. Limit of detection, 2–10 mg/L [Bjornstad et al. 2009]. Column: Brownlee O Spheri-5 RP-18 (100 Â 1.0 mm i.d., 5 mm). Mobile phase: methanol : water (50 : 50) with 0.2% formic acid, flow rate 40 mL/min.
• ESI, MRM acquisition mode. Limit of detection, 0.1 mg/L [Forsstrom et al. 2001].

IR - Infrared

(Solid) DMT IR Spectra

Other IR data (Clarke's second): Principal peaks at wavenumbers 743, 1113, 1235, 1050, 812, 1010 (KBr disk)

UV-Vis

DMT UV Spectra

Other UV-Vis data:

• λmax 222nm (log e 4.48), 277 (3.77) and 288 (3.75) Ghosal et al 1969
• λmax 222-224, 274 & 294nm Banergee & Ghosal 1969
• λmax 222, 277, 287 & 294 nm Ghosal & Banergee 1969
• λmax 274, 283, 291nm (refernce material) 275, 283, 291nm (isolated material) Fish et al 1955
• λmax (CH3OH): 220, 280, 290 (= 5500, 5600, 5000) De Moraes et al 1990
• λmax (EtOH): 226, 275 (sh), 279, 284, 293nm Grina et al 1982
• λmax 276, 282, 290nm

λmin 278, 287nm Martin & Alexander 1968

• λmax 275, 219 (0.1N NaOH)
• λmax 290, 276, 282 (EtOH) Sunshine 1981
• λmax of Xanthydrol reactive product (CHCl3): 510nm

λmin of Xanthydrol reactive product (CHCl3): 400nm Gander et al 1976

• Quantification. Average between: Ab@238/737*10000 = X ug/ml

Ab@308/296.1*10000 = X ug/ml

NMR

  

(NMR info source, method description and results discussion:Microgram bulletin volume 5, n14, pg6 )

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Scientific publications

• Scientific Articles on Psychedelics WIKI
• Scientific Articles thread

Links of interest

• http://en.wikipedia.org/wiki/Dimethyltryptamine
• http://www.erowid.org/chemicals/dmt/dmt.shtml

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