Ammonia → HCID 178489931, Verbindung

HRID 1663004Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1663004
[CH:1]([C@H:4]1[CH2:9][CH2:8][C@H:7]([NH2:10])[CH2:6][CH2:5]1)([CH3:3])[CH3:2].[CH:11]1[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH:14]=[N:13][N:12]=1.C[CH2:22][O:23][C:24]([CH3:26])=O.[NH3:27]>O>[CH:1]([C@H:4]1[CH2:9][CH2:8][C@H:7]([NH:10][C:11]2[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[C:14]([CH2:4][C:1]3[CH:2]=[N:27][C:24]([O:23][CH3:22])=[CH:26][CH:3]=3)=[N:13][N:12]=2)[CH2:6][CH2:5]1)([CH3:3])[CH3:2]

Komponenten

6

Edukt 4

HCID 222AmmoniaHCID 8857Ethyl AcetateHCID 9207PhthalazineHCID 178448118HCID 178448118, Verbindung

Produkt 1

HCID 178489931HCID 178489931, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Under N2 atmosphere, in an ampoule 1.8 g (12.7 mMol) of trans 4-isopropyl-cyclohexylamine (preparation see Arzneim. Forsch. 1969, 19, 140) and 700 mg (2.4 mMol) of 1-chloro-4-[6-methoxy-pyridin-3-yl)methyl]phthalazine are heated during 14 h at 140° C. The suspension is dissolved by dilution with EtOAc, 1.5 ml of NH3 solution (25%) and water, and the aqueous phase is removed and extracted twice with EtOAc. The organic phases are washed with water and brine, dried (Na2SO4) and evaporated. Crystallization from EtOAc/hexane 1:1 results in the title compound: M.p. 124-125° C.; FAB-MS: (M+H)+=391; HPLC(Grad20-100) tRet12.4.

Aufarbeitung

  1. customthe aqueous phase is removed
  2. extractionextracted twice with EtOAc
  3. washThe organic phases are washed with water and brine
  4. dry with materialdried (Na2SO4)
  5. customevaporated
  6. customCrystallization from EtOAc/hexane 1:1

Quellen und Nachweise

ORD-Eintrag
ord-4ceb48b07d4646b3bb1e98cfb54e0d38
Quelldatensatz
uspto-grants-2011_10
Patentnummer
US08034814B2

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