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Saturday 28 February 2015

Atorvastatin calcium


Atorvastatin calcium




1H NMR DMSOD6






13C NMR DMSOD6



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http://www.google.com/patents/EP0848705B1?cl=en

    SOLID STATE NUCLEAR MAGNETIC RESONANCE (NMR)Methodology
  • [0028]
    All solid-state 13C NMR measurements were made with a Bruker AX-250, 250 MHz NMR spectrometer. High resolution spectra were obtained using high-power proton decoupling and cross-polarization (CP) with magic-angle spinning (MAS) at approximately 5 kHz. The magic-angle was adjusted using the Br signal of KBr by detecting the side bands as described by Frye and Maciel (Frye J.S. and Maciel G.E., J. Mag. Res., 1982;48:125). Approximately 300 to 450 mg of sample packed into a canister-design rotor was used for each experiment. Chemical shifts were referenced to external tetrakis (trimethylsilyl)silane (methyl signal at 3.50 ppm) (Muntean J.V. and Stock L.M., J. Mag. Res., 1988;76:54).
  • [0029]
    Table 2 shows the solid-state NMR spectrum for crystalline Form I atorvastatin hydrate.
    Figure 00120001
    Carbon Atom Assignment and Chemical Shift for Form I Atorvastatin hydrate
    Assignment (7 kHz)Chemical Shift
    C12 or C25182.8
    C12 or C25178.4
    C16166.7 (broad) and 159.3
    Aromatic Carbons
    C2-C5, C13-C18, C19-C24, C27-C32137.0
    134.9
    131.1
    129.5
    127.6
    123.5
    120.9
    118.2
    113.8
    C8,C1073.1
    70.5
    68.1
    64.9
    Methylene Carbons
    C6, C7, C9, C1147.4
    41.9
    40.2
    C3326.4
    25.2
    C3421.3




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http://www.google.co.in/patents/US7834195
EXAMPLE 1 Preparation of atorvastatin calcium propylene glycol solvate under anhydrous conditions
Atorvastatin calcium (5 g) was dissolved in racemic propylene glycol followed by the addition of 7 parts of ethyl acetate. The resulting mixture was warmed to 55-60° C. and stirred for 8-10 hours to afford a white suspension. The suspension was cooled to 20-25° C. and filtered to provide 3.3 g of atorvastatin calcium propylene glycol solvate after drying under vacuum at 50-60° C. Propylene glycol content: 6% by NMR.
Isopropyl acetate and methyl, isobutyl ketone (MIBK) can also be used in the example 1 procedure.
The DSC and IR of the solvate made in this example is shown in FIGS. 1 and 2, respectively.
1H-NMR(DMSO-d6): δ 9.82 (s, 1H), 7.51 (ad, J=8.0 Hz, 2H), 7.33-7.11 (m, 6H), 7.08-6.95 (m, 6H), 5.93 (bs, 1H), 4.76 (bs, 1H), 4.65-4.33 (m, 1H), 4.09-3.85 (m, 1H), 3.84-3.68 (m, 2H), 3.62-3.44 (m, 1.5H), 3.30-3.09 (m, 2H), 2.08 (dd, J=15.4, 3.7 Hz), 1.97 (dd, J=15.3, 8.0 Hz), 1.71-1.50 (m, 2H), 1.50-1.31 (m, 7H), 1.30-1.11 (m, 1H), 1.00 (d, J=6.3 Hz, 1.5H).




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http://www.google.st/patents/US20040054193




urther, the present invention is directed to crystalline Form V atorvastatin and hydrates thereof characterized by the following solid-state 13C nuclear magnetic resonance (ssNMR) spectrum wherein chemical shift is expressed in parts per million:
AssignmentChemical Shift
C12 or C25185.7
C12 or C25176.8
C16166.9
Aromatic Carbons138.7
C2-C5, C13-C18,136.3
C19-C24, C27-C32
133.0
128.4
122.0
117.0
116.3
C8, C1068.0
Methylene Carbons43.1
C6, C7, C9, C11
C3325.6
C3419.9
[0017] Additionally, the present invention is directed to crystalline Form V atorvastatin and hydrates thereof characterized by the following Raman spectrum having peaks expressed in cm−1:

3062
1652
1604
1528
1478
1440
1413
1397
1368
1158
1034
1001
825
245
224
130
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