Water → N-cyclopropylpyridin-4-amine

HRID 255449Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 255449
Cl[C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[CH:15]1([NH2:18])[CH2:17][CH2:16]1.O>CN(C=O)C>[CH:15]1([NH:18][C:2]2[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=2)[CH2:17][CH2:16]1

Komponenten

6

Edukt 4

HCID 962WaterHCID 8471TriethylamineHCID 122884-ChloropyridineHCID 69828Cyclopropylamine

Produkt 1

HCID 19854218N-cyclopropylpyridin-4-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a magnetically stirred, 25° C. solution of 2.3 g (0.006 mol) of product of Step A and 0.71 g (0.007 mol) of triethylamine in 40 ml of DMF was added dropwise 0.38 g (0.007 mol) of cyclopropylamine. After 18 hours the reaction mixture was poured into H2O and extracted with diethyl ether. The ether phase was washed with H2O, and dried (MgSO4). The dry ether phase was concentrated in vacuo to 1.95 g of a brown solid. The crude was recrystallized from hexane/EtOAc affording 1.2 g (50%) of product as a beige solid; mp 111`-112° C.

Aufarbeitung

  1. extractionextracted with diethyl ether
  2. washThe ether phase was washed with H2O
  3. dry with materialdried (MgSO4)
  4. concentrationThe dry ether phase was concentrated in vacuo to 1.95 g of a brown solid
  5. customThe crude was recrystallized from hexane/EtOAc affording 1.2 g (50%) of product as a beige solid
  6. custom-112° C.

Quellen und Nachweise

ORD-Eintrag
ord-8b59ca97589243eb838752504535a307
Quelldatensatz
uspto-grants-1987_10
Patentnummer
US04698093

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