Ammonium Chloride → HCID 178455675, Verbindung

HRID 603002Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 603002
[C:1]1([CH:7]([N:14]2[CH2:17][CH:16]([CH:18]([C:23]3[CH:24]=[C:25]([CH:28]=[C:29]([F:31])[CH:30]=3)[C:26]#[N:27])[C:19]([F:22])([CH3:21])[CH3:20])[CH2:15]2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[N-:32]=[N+:33]=[N-:34].[Na+].[Cl-].[NH4+]>CN(C=O)C>[C:1]1([CH:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:14]2[CH2:15][CH:16]([CH:18]([C:23]3[CH:24]=[C:25]([C:26]4[NH:34][N:33]=[N:32][N:27]=4)[CH:28]=[C:29]([F:31])[CH:30]=3)[C:19]([F:22])([CH3:21])[CH3:20])[CH2:17]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

Komponenten

5

Edukt 3

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 113390333-{1-[(Diphenylmethyl)azetidin-3-yl]-2-fluoro-2-methylpropyl}-5-fluorobenzonitrile

Produkt 1

HCID 178455675HCID 178455675, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A mixture of 1.17 g (2.81 mmol) of 3-{1-[(diphenylmethyl)azetidin-3-yl]-2-fluoro-2-methylpropyl}-5-fluorobenzonitrile, 914 mg (14.06 mmol) of sodium azide, and 715 mg (14.05 mmol) of ammonium chloride in 15 mL of DMF was stirred for 16 h. Then it was concentrated to remove solvents. The residue was purified by silica gel chromatography with CH2Cl2/MeOH/NH3 (2M) in MeOH to afford the title compound as a white solid;

Aufarbeitung

  1. concentrationThen it was concentrated
  2. customto remove solvents
  3. customThe residue was purified by silica gel chromatography with CH2Cl2/MeOH/NH3 (2M) in MeOH

Quellen und Nachweise

ORD-Eintrag
ord-1036100b0da14d0592a682ab575adb13
Quelldatensatz
uspto-grants-2011_03
Patentnummer
US07906652B2

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