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Hydrochloric Acid → 4-chloro-6-(3-isopropyl-1-methyl-1H-pyrazol-5-yl)-2-(3-methyl-1H-indol-4-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine

HRID 80814
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 80814
[CH:1]([C:4]1[CH:8]=[C:7]([N:9]2[CH2:39][CH2:38][C:12]3[N:13]=[C:14]([C:18]4[CH:26]=[CH:25][CH:24]=[C:23]5[C:19]=4[C:20]([CH3:37])=[CH:21][N:22]5S(C4C=CC(C)=CC=4)(=O)=O)[N:15]=[C:16](O)[C:11]=3[CH2:10]2)[N:6]([CH3:40])[N:5]=1)([CH3:3])[CH3:2].[OH-].[K+].[OH-].[NH4+].Cl.C([O-])(O)=O.[Na+].P(Cl)(Cl)([Cl:53])=O>CO.CC(C)=O.O>[Cl:53][C:16]1[C:11]2[CH2:10][N:9]([C:7]3[N:6]([CH3:40])[N:5]=[C:4]([CH:1]([CH3:2])[CH3:3])[CH:8]=3)[CH2:39][CH2:38][C:12]=2[N:13]=[C:14]([C:18]2[CH:26]=[CH:25][CH:24]=[C:23]3[C:19]=2[C:20]([CH3:37])=[CH:21][NH:22]3)[N:15]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

10

Edukt 6

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 14923Ammonium HydroxideHCID 24813Phosphorus oxychlorideHCID 516892Sodium Bicarbonate2×HCID 178427365HCID 178427365, Verbindung

Produkt 1

HCID 86690264
4-chloro-6-(3-isopropyl-1-methyl-1H-pyrazol-5-yl)-2-(3-methyl-1H-indol-4-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 180AcetoneLösungsmittelHCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

To a solution of 6-(3-isopropyl-1-methyl-1H-pyrazol-5-yl)-2-(3-methyl-1-tosyl-1H-indol-4-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-ol (550 mg, 0.988 mmol) in methanol (5 mL) in a microwave vial, was added potassium hydroxide (554 mg, 9.88 mmol) and then 28% ammonium hydroxide (1 mL, 0.988 mmol). The reaction was heated at 80° C. via microwave irradiation for 45 min. The reaction mixture was poured into iced water, then 4 N aq HCl was added to acidify the reaction mixture to pH=1, then NaHCO3 solid was added to neutralize reaction mixture to pH=7-8. The mixture was extracted twice with a solution of 5% trifluoroethanol in DCM. The combined organic layers were washed with brine, dried over Na2SO4, filtered and concentrated. The resulting residue was dissolved in dichloroethane (3 mL), and the reaction flask was charged with phosphorus oxychloride (3.67 mL, 39.5 mmol). The reaction flask was capped and then heated to 80° C. for 1 h. The reaction mixture was cooled to r.t. and poured into ice water and diluted with acetone (10 mL). The reaction mixture was stirred for 30 min to provide a clear solution. At that point, NaHCO3 solid was added to neutralize the reaction, and the mixture was extracted twice with DCM. The resulting residue was purified via silica gel FCC (0-100% EtOAc/heptane) to provide 4-chloro-6-(3-isopropyl-1-methyl-1H-pyrazol-5-yl)-2-(3-methyl-1H-indol-4-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine. MS (ESI+) m/z 421.2 (M+H)+.

Aufarbeitung

  1. extractionThe mixture was extracted twice with a solution of 5% trifluoroethanol in DCM
  2. washThe combined organic layers were washed with brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. dissolutionThe resulting residue was dissolved in dichloroethane (3 mL)
  7. customThe reaction flask was capped
  8. temperatureheated to 80° C. for 1 h
  9. temperatureThe reaction mixture was cooled to r.t.
  10. customto provide a clear solution
  11. customthe reaction
  12. extractionthe mixture was extracted twice with DCM
  13. customThe resulting residue was purified via silica gel FCC (0-100% EtOAc/heptane)

Quellen und Nachweise

ORD-Eintrag
ord-fa4f83bd4f994f3a98d908054b4bd60c
Quelldatensatz
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08846656B2

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