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Thursday 1 January 2015

13C {1H} INVGATE



Spectra of the nuclei X decoupled from protons, but without signal amplification due to the nuclear Overhauser effect. In this case, the integral intensities of the signals is proportional to the amount of the corresponding nuclei H.

Spectra of the nuclei X decoupled from protons, where X - the core of the band 31 P- 15 N or 19 F. Provide information on the chemical shifts and the integrated intensity of the signal for the nuclei X.







tbilisi georgia






































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HXCORR




HXCORR



Spectra of the nuclei X decoupled from protons, where X - the core of the band 31 P- 15 N or 19 F. Provide information on the chemical shifts for nuclei X.


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1 H {X}




The spectra of 1 H and 1 H {X} (isolated from nuclei with X, where X - core from the range of 31 P- 109 Ag).Provide information on the chemical shifts and the values ​​of the constants of spin-spin coupling J HH , as well as the integrated intensity of the signal for the nuclei 1 H.








DER OF ISATIN






Isatin (1H-indole-2,3-dione) is an endogenous natural compound under intense development in medicinal chemistry. Here, we characterize isatin Schiff base derivative by X-ray crystallography. We describe a derivative that crystallizes E-isomer form in the triclinic space group P1; a=5.9580 (4) Ã…, b=8.4184 (7) Ã…, c=14.1801 (14) Ã…, α = 73.962 (8)°, β =83.184 (7)°, γ = 81.143 (6)°. NMR data show that E-conformer interconverts to the Z-conformer when dissolved, this equilibrium weakly depends on the solvent type. The Z-isomer geometry and the energetics of ΔEE-Z interconversion barriers were determined by quantum chemical calculations. The isomers are further characterized by means of FT-IR and UV-Vis spectroscopy.




Chloroindolo[2.1 -b]quinazoline-6.12-dione

Chloroindolo[2.1 -b]quinazoline-6.12-dione
Figure imgf000027_0002
Using the procedure in Example 12, and substituting NMP for DMF and isatin for 5-fluoroisatin gave 53 mg (7%) of the title compound: mp 320°C (dec); 

lH NMR(DMSO-d6) δ 7.46-7.54 (m, IH), 7.86-7.92 (m, 3H), 8.26-8.28 (m, IH), 8.45-8.50 (m, 2H); 

MS (M+H)+ 282.

5-methoxyisatin


Figure imgf000023_0002


5-methoxyisatin

To a stirred solution of 12.6 g (75.6 mmol) of chloral hydrate in 168 mL water was added the following: 180 g (1.27 mole) sodium sulfate; 7.67 g (62.4 mmol) 4-methoxyaniline in 6 mL of concentrated HC1 and 42 mL of water; and 15.4 g (224 mmol) of hydroxylamine hydrochlori.de in 70 mL of water. The mixture was heated slowly to 100°C and kept at that temperature for 1 h. The mixture was cooled to room temperature, filtered and the precipitate washed with water and dried to give 81% yield of the anilide: Η MR (300 MHz, DMSO-d6) δ 12.15 (s, IH) 10.1 (s, IH) 7.65 (s, IH) 7.6 (d, 2H) 6.95 (d, 2H) 3.75 (s, 3H). The crude anilide (10.8 g, 61 mmol) was added to 27 mL of concentrated sulfuric acid at 50°C, heated at 65°C for 1 h, cooled to room temperature, and poured into 300 mL of ice. The solids were filtered and dried in vacuo over P2O5. The crude isatin was dissolved in boiling CH2C12 with 2% N-methylpyrrolidone and applied to a silica gel column. The product was eluted using a CH2Cl2:MeOH gradient 100% CH2C12 to (9:1) CH2Cl2:MeOH. 5-Methoxyisatin was obtained in 12% yield overall: mp 168-172°C;

 *H NMR (300 MHz, DMSO-d6) δ 10.85 (s, IH) 7.17-7.24 (m, IH) 7.1 (d, IH) 6.87 (d, IH) 3.75 (s, 3H); 


MS (M+CH4CN)+ 158.

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5-fluoro-6-(4-methylpiperazinyl isatin


Figure imgf000022_0002
To a solution of 5,6-difluoroisatin (1.0 g, 5 mmol) in 50 mL of dimethyl sulfoxide was added N-methylpiperazine (5.47 g, 50 mmol). The mixture was stirred for 4 h at room temperature and the crude reaction mixture was diluted with ethyl acetate. The organic solution was washed with saturated sodium bicarbonate. The organic layers were separated and concentrated to give the title compound in 72% yield: mp 150°C (dec); 

1H NMR (300 MHz, DMSO-d6) δ 10.8 (br s, IH), 7.3 (d, IH), 6.4 (d, IH), 2.25 (s, 3H), 2.2 (m, 4H), 2.1 (m, 4H)

N CHLORO ISATIN













http://www.scielo.br/scielo.php?pid=S0103-50532011000200010&script=sci_arttext


Journal of the Brazilian Chemical Society

Print version ISSN 0103-5053

J. Braz. Chem. Soc. vol.22 no.2 São Paulo Feb. 2011

http://dx.doi.org/10.1590/S0103-50532011000200010 






Spectroscopic data








1a: IR (film) Î½ max/cm-1: 3085, 2923, 1764, 1729, 1614, 1596, 1483, 1315, 1294, 1176, 1126, 950, 427. 












1H NMRδ (200 MHz, CDCl3): 3.23 (3H, s), 6.85 (1H, d, 8.0 Hz), 7.51-7.57 (2H, m); 







13C NMR Î´ (50 MHz, CDCl3): 26.5 (CH3), 111.4 (CH), 118.3 (q), 125.2 (CH), 129.7 (q), 137.9 (CH), 149.8 (q), 157.8 (q), 182.4 (q); 









MS (70 eV)m/z 195 [M] +, 197 [M+2] +, 160, 104.