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3-Aminobenzoic Acid → Ammonia methanol

HRID 2370949
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2370949
Cl.ClC1N=C(NC2CC(C)(C)NC(C)(C)C2)C(F)=C[N:4]=1.[CH:21]1([C:24]2[C:29]([N:30]3[CH:34]=[N:33][N:32]=[N:31]3)=[CH:28][C:27]([NH2:35])=[C:26]([F:36])[CH:25]=2)[CH2:23][CH2:22]1.N1C=NN=N1.Cl[C:43]1[N:48]=[C:47]([NH:49][CH:50]2[CH2:55][C:54]([CH3:57])([CH3:56])[NH:53][C:52]([CH3:59])([CH3:58])[CH2:51]2)[C:46]([F:60])=[CH:45][N:44]=1.NC1C=C(C=CC=1)[C:65](O)=[O:66].N1C=CC=NC=1>CC(O)C>[NH3:4].[CH3:65][OH:66].[CH:21]1([C:24]2[C:29]([N:30]3[CH:34]=[N:33][N:32]=[N:31]3)=[CH:28][C:27]([NH:35][C:43]3[N:48]=[C:47]([NH:49][CH:50]4[CH2:51][C:52]([CH3:58])([CH3:59])[NH:53][C:54]([CH3:57])([CH3:56])[CH2:55]4)[C:46]([F:60])=[CH:45][N:44]=3)=[C:26]([F:36])[CH:25]=2)[CH2:23][CH2:22]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 6

HCID 74193-Aminobenzoic AcidHCID 9260PyrimidineHCID 58065786HCID 58065786, VerbindungHCID 59442725HCID 59442725, VerbindungHCID 86653878HCID 86653878, VerbindungHCID 178418441HCID 178418441, Verbindung

Produkt 2

HCID 21705897
Ammonia methanol
Ausbeute 1 %
HCID 56644100HCID 56644100, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

A mixture of 2-chloro-5-fluoro-N-(2,2,6,6-tetramethylpiperidin-4-yl)pyrimidin-4-amine hydrochloride (6.68 g, 20.68 mmol, 1 equiv), 4-cyclopropyl-2-fluoro-5-(1H-tetrazol-1-yl)benzenamine (6.80 g, 31.02 mmol, 1.5 equiv), and PTSA monohydrate (3.15 g, 16.54 mmol, 0.8 equiv) in IPA (200 mL) were heated to 70° C. for 4 days. LCMS indicated 2-4% of the cleaved tetrazole product and 7-9% unreacted 2-chloro-5-fluoro-N-(2,2,6,6-tetramethylpiperidin-4-yl)pyrimidin-4-amine. After cooling the reaction mixture to ambient temperature, 3-amino benzoic acid (8.51 g, 62.04 mmol, 3 equiv) was added and heated to 70° C. for overnight to scavenge the unreacted pyrimidine. After cooling to ambient temperature, the crude mixture was concentrated to dryness. The residue was taken in ice-cold water and EtOAc then adjusted to ca. pH 12-14 with 1N NaOH (300 mL). The aqueous and organic layers were partitioned, and the organic layer washed with 1N NaOH (2×300 mL). The aqueous layer was extracted with EtOAc (1×150 mL). The combined organic extracts were dried (Na2SO4), filtered, and the solvent removed under vacuum. The crude product was purified by flash chromatography and eluted with DCM:2M NH3/MeOH=100:0 to 96:4 using 1% 2M NH3/MeOH increments to provide the desired product which was triturated with EtOAc/hexane to give the title compound (5.16 g, 53%) as a solid.

Aufarbeitung

  1. temperatureAfter cooling the reaction mixture to ambient temperature
  2. temperatureheated to 70° C. for overnight
  3. temperatureAfter cooling to ambient temperature
  4. concentrationthe crude mixture was concentrated to dryness
  5. customThe aqueous and organic layers were partitioned
  6. washthe organic layer washed with 1N NaOH (2×300 mL)
  7. extractionThe aqueous layer was extracted with EtOAc (1×150 mL)
  8. dry with materialThe combined organic extracts were dried (Na2SO4)
  9. filtrationfiltered
  10. customthe solvent removed under vacuum
  11. customThe crude product was purified by flash chromatography
  12. washeluted with DCM

Quellen und Nachweise

ORD-Eintrag
ord-83f95e61ebe04fbb8b900c478585a459
Quelldatensatz
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08710223B2

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