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.
  

  

  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
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:

	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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