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






































////////////

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.


vietnam

.


 



 
 

 
 

 

 dalat city
hanoi











//////////

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) Å, b=8.4184 (7) Å, c=14.1801 (14) Å, 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.

Journal of Molecular Structure, 2014

P.B. Davidovich, D.S. Novikova, V.G. Tribulovich, S.N. Smirnov, V.V. Gurzhiy, G. Melino, A.V. Garabadzhiu

”First X-ray Structural Characterization of Isatin Schiff-Base Derivative. NMR and Theoretical Conformational Studies”

Journal of Molecular Structure, 2014, 1075, 450-455

DOI: 10.1016/j.molstruc.2014.07.008

Chloroindolo[2.1 -b]quinazoline-6.12-dione

Chloroindolo[2.1 -b]quinazoline-6.12-dione

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.

http://www.google.com/patents/WO1995013807A1?cl=en

5-methoxyisatin

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.

vietnam

.


 



 
 

 
 

 

 dalat city
hanoi











//////////



 DRUG APPROVALS BY DR ANTHONY MELVIN CRASTO .....FOR BLOG HOME CLICK HERE

Join me on Linkedin

Join me on Facebook FACEBOOK

Join me on twitter     

Join me on google plus Googleplus

 amcrasto@gmail.com

5-fluoro-6-(4-methylpiperazinyl isatin

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)