Atorvastatin calcium
1H NMR DMSOD6
13C NMR DMSOD6
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http://www.google.com/patents/EP0848705B1?cl=en
- [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.
Carbon Atom Assignment and Chemical Shift for Form I Atorvastatin hydrate Assignment (7 kHz) Chemical Shift C12 or C25 182.8 C12 or C25 178.4 C16 166.7 (broad) and 159.3 Aromatic Carbons C2-C5, C13-C18, C19-C24, C27-C32 137.0 134.9 131.1 129.5 127.6 123.5 120.9 118.2 113.8 C8,C10 73.1 70.5 68.1 64.9 Methylene Carbons C6, C7, C9, C11 47.4 41.9 40.2 C33 26.4 25.2 C34 21.3
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http://www.google.co.in/patents/US7834195
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).
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:
Assignment | Chemical Shift | ||
C12 or C25 | 185.7 | ||
C12 or C25 | 176.8 | ||
C16 | 166.9 | ||
Aromatic Carbons | 138.7 | ||
C2-C5, C13-C18, | 136.3 | ||
C19-C24, C27-C32 | |||
133.0 | |||
128.4 | |||
122.0 | |||
117.0 | |||
116.3 | |||
C8, C10 | 68.0 | ||
Methylene Carbons | 43.1 | ||
C6, C7, C9, C11 | |||
C33 | 25.6 | ||
C34 | 19.9 | ||
[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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