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Hydrochloric Acid → HCID 68452746, Verbindung

HRID 2357649
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2357649
[C:1]([C:3]1[C:12]2[C:7](=[CH:8][C:9]([C:13]3[CH:14]=[C:15]([CH:20]=[CH:21][C:22]=3[CH3:23])[C:16](OC)=[O:17])=[CH:10][CH:11]=2)[CH:6]=[N:5][N:4]=1)#[N:2].Cl.[CH:25]1([NH2:28])[CH2:27][CH2:26]1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>C(OCC)(=O)C.CN(C=O)C>[C:1]([C:3]1[C:12]2[C:7](=[CH:8][C:9]([C:13]3[CH:14]=[C:15]([CH:20]=[CH:21][C:22]=3[CH3:23])[C:16]([NH:28][CH:25]3[CH2:27][CH2:26]3)=[O:17])=[CH:10][CH:11]=2)[CH:6]=[N:5][N:4]=1)#[N:2]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 69828CyclopropylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 68455479HCID 68455479, Verbindung

Produkt 1

HCID 68452746HCID 68452746, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittel
HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

To methyl 3-(1-cyanophthalazin-6-yl)-4-methylbenzoate (0.800 g, 2.6 mmol) was added 6N HCl (10.6 mL) and the reaction was heated in a microwave oven for 25 min at 120° C. The reaction was concentrated, dried in vacuo and DMF (5.3 mL) and cyclopropylamine (0.92 mL, 13 mmol) were added. HATU (2.0 g, 5.3 mmol) was added and the reaction mixture was stirred at RT for 1 h, then diluted with 75 mL ethyl acetate, partitioned with sodium bicarbonate (saturated, aqueous), and the organic layers were washed 2×20 mL with sodium bicarbonate (saturated, aqueous), separated, dried over sodium sulfate, concentrated in vacuo, and purified by HPLC to give the title compound. MS (ES+): 329(M+H)+.

Aufarbeitung

  1. concentrationThe reaction was concentrated
  2. additionwere added
  3. custompartitioned with sodium bicarbonate (saturated, aqueous)
  4. washthe organic layers were washed 2×20 mL with sodium bicarbonate (saturated, aqueous)
  5. customseparated
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated in vacuo
  8. custompurified by HPLC

Quellen und Nachweise

ORD-Eintrag
ord-15ac612c413d4d75886c89582ee75fdc
Quelldatensatz
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07759337B2

Notizen zur Reaktion

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