Nitrilotriacetic Acid Anhydride,1H NMR AND 13C NMR

learn nmr the simple way with simple molecules, two-four signals at a time with examples

PROTON NMR

1H(d6-acetone, 400 MHz): 

3.920(s, 4H), 
The two PLUS two  NCH2 protons of -NCH2-C=O-O on the ring

3.620(s, 2H); 

The two   NCH2 protons of -NCH2-C=O-OH on side chain


CARBON 13 NMR


13C(d6-acetone, 100 MHz): 

171.18, The single carbonyl carbon  of -NCH2-C=O-OH on side chain

165.51(2C),  The two  carbonyl carbons  of -NCH2-C=O- on the ring

54.79, The single N attached carbon  of -NCH2-C=O-OH on side chain

52.54(2C), The two N attached Carbons at   -NCH2-C=O-O on the ring




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MIDOSTAURIN MP

MIDOSTAURIN
https://www.google.co.in/patents/US5093330
EXAMPLE 18 N-benzoyl-staurosporine

0.035 ml (0.3 mmol) of benzoyl chloride is added at room temperature to a solution of 116.5 mg (0.25 mmol) of staurosporine and 0.065 ml (0.38 mmol) of N,N-diisopropylethylamine in 2 ml of chloroform and the whole is stirred for 10 minutes. The reaction mixture is diluted with chloroform, washed with sodium bicarbonate solution, dried over magnesium sulphate and concentrated by evaporation. The crude product is chromatographed on silica gel (eluant:methylene chloride/ethanol 30:1); m.p. 235


SEE FULL REPORT ON
http://www.allfordrugs.com/2014/01/14/midostaurin-with-potential-antiangiogenic-and-antineoplastic-activities/

IDELALISIB NMR

Idelalisib

An antineoplastic agent and p110delta inhibitor

(S)-2-(1-(9H-purin-6-ylamino)propyl)-5-fluoro-3-phenylquinazolin-4(3H)-one

Icos (Originator)

• CAL-101
• GS-1101
• Idelalisib
• UNII-YG57I8T5M0

M.Wt: 415.43
Formula: C22H18FN7O

CAS No.: 870281-82-6
CAL-101 Solubility: DMSO ≥80mg/mL Water <1.2mg/mL Ethanol ≥33mg/mL

5-Fluoro-3-phenyl-2-[(1S)-1-(7H-purin-6-ylamino)propyl]-4(3H)-quinazolinone

 WO2005113556A1
compound 107 idelalisib as a light yellow solid (7.2 g, 50%).

1H NMR (300 MHz, 80 0C, DMSO-d5) δ 12.66 (broad s, IH), 8.11 (s, IH), 8.02 (broad s, IH), 7.81-7.73 (m, IH),7.60-7.42 (m, 6H), 7.25-7.15 (m, 2H), 4.97 (broad s, IH), 2.02-1.73 (m, 2H), 0.79 (t, J= 7.3 Hz, 3H).

ESI-MS m/z 416.2 (MH+).

C, H, N elemental analysis (C22Hi8N7OF-EtOH- 0.4 H2O).

Chiral purity 99.8:0.2 (S:R) using chiral HPLC (4.6 x 250 mm Chiralpak ODH column, 20 °C, 85:15 hexanes : EtOH, 1 rnL/min, sample loaded at a concentration of 1 mg/mL in EtOH) . The reaction described above and compound 107 idelalisib are shown below.

WO2005113556A1

The synthesis of a compound in accordance with formula I is first exemplified using steps A-E below, which provide a synthetic procedure for compound 107, the structure of which is shown below.

(107) is idelalisib

.................
READ AT
 http://newdrugapprovals.wordpress.com/2014/01/14/idelalisib-us-fda-accepts-nda-for-gileads-idelalisib-for-the-treatment-of-refractory-indolent-non-hodgkins-lymphoma/

New Short Strategy for the Synthesis of the Dibenz[b,f]oxepin Scaffold | ORGANIC CHEMISTRY SELECT

New Short Strategy for the Synthesis of the Dibenz[b,f]oxepin Scaffold | ORGANIC CHEMISTRY SELECT:

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New Short Strategy for the Synthesis of the Dibenz[b,f]oxepin Scaffold | ORGANIC CHEMISTRY SELECT

New Short Strategy for the Synthesis of the Dibenz[b,f]oxepin Scaffold | ORGANIC CHEMISTRY SELECT:

'via Blog this'

see spectral discussions