Diethylamine → Diethylamine

HRID 71013

Reaktionsgleichung

Reaktionsgleichung von HRID 71013
[CH2:1]([NH:3][CH2:4][CH3:5])[CH3:2].[CH3:6][CH:7]([C:9]1[N:13]([CH2:14][CH2:15][C@@H:16]([OH:24])[CH2:17][C@@H:18]([OH:23])[CH2:19][C:20]([OH:22])=[O:21])[C:12]([C:25]2[CH:26]=[CH:27][C:28]([F:31])=[CH:29][CH:30]=2)=[C:11]([C:32]2[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=2)[C:10]=1[C:38]([NH:40][C:41]1[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=1)=[O:39])[CH3:8]>C(#N)C>[CH2:1]([NH:3][CH2:4][CH3:5])[CH3:2].[CH3:8][CH:7]([C:9]1[N:13]([CH2:14][CH2:15][C@@H:16]([OH:24])[CH2:17][C@@H:18]([OH:23])[CH2:19][C:20]([OH:22])=[O:21])[C:12]([C:25]2[CH:30]=[CH:29][C:28]([F:31])=[CH:27][CH:26]=2)=[C:11]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[C:10]=1[C:38]([NH:40][C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1)=[O:39])[CH3:6].[CH2:1]([NH:3][CH2:4][CH3:5])[CH3:2]

Komponenten

5

Edukt 2

HCID 8021DiethylamineHCID 60823Atorvastatin3×

Produkt 2

HCID 8021DiethylamineHCID 11556397Atorvastatin diethylamine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel3×

Versuchsvorschrift

The diethylamine salt of atorvastatin (Form A) was synthesized by preparing a stock solution of the free acid of atorvastatin (U.S. Pat. No. 5,273,995) in acetonitrile (1 g in 40 mL of ACN). A solution of diethylamine was prepared by dissolving 132.33 mg (1.0 equivalents) in acetonitrile (20 mL). The stock solution of atorvastatin free acid was added to the counterion solution with stirring. Over time, an additional 40 mL of acetonitrile was added to prevent the formation of a gel. After 5 days of stirring at ambient temperature, the solids were isolated by vacuum filtration using a Buchner funnel fitted with a paper filter (#2 Whatman). The solids were rinsed with acetonitrile (75 mL), and placed in a 25° C. oven under nitrogen to dry overnight to afford atorvastatin diethylamine Form A.

Aufarbeitung

  1. stirringAfter 5 days of stirring at ambient temperature
  2. customthe solids were isolated by vacuum filtration
  3. customfitted with a paper
  4. filtrationfilter (#2 Whatman)
  5. washThe solids were rinsed with acetonitrile (75 mL)
  6. customplaced in a 25° C.
  7. customto dry overnight

Quellen und Nachweise

ORD-Eintrag
ord-36de434695f84921a6b84d658f29faa3
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08822703B2

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