Ammonium Chloride → HCID 178433654, Verbindung

HRID 2234006Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2234006
[Cl:1][C:2]1[C:6]([Cl:7])=[C:5]([CH3:8])[NH:4][C:3]=1[C:9]([NH:11][CH:12]1[CH2:17][CH2:16][N:15]([C:18]2[S:19][C:20]([C:23]#[N:24])=[CH:21][N:22]=2)[CH2:14][CH2:13]1)=[O:10].[N-:25]=[N+:26]=[N-:27].[Na+].[Cl-].[NH4+]>CN(C=O)C>[Cl:1][C:2]1[C:6]([Cl:7])=[C:5]([CH3:8])[NH:4][C:3]=1[C:9]([NH:11][CH:12]1[CH2:17][CH2:16][N:15]([C:18]2[S:19][C:20]([C:23]3[NH:27][N:26]=[N:25][N:24]=3)=[CH:21][N:22]=2)[CH2:14][CH2:13]1)=[O:10]

Komponenten

5

Edukt 3

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 68580052HCID 68580052, Verbindung

Produkt 1

HCID 178433654HCID 178433654, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

To a solution of 3,4-dichloro-N-[1-(5-cyano-1,3-thiazol-2-yl)piperidin-4-yl]-5-methyl-1H-pyrrole-2-carboxamide (Example 321, 0.100 g, 0.26 mmol) in DMF (3 ml) was added sodium azide (0.169 g, 2.60 mmol) followed by the addition of ammonium chloride (0.139 g, 2.60 mmol) at room temperature. The reaction was stirred at 120° C. for 3 hrs. The reaction mixture was cooled to room temperature, filtered and purified by reverse phase HPLC eluting with acetonitrile/water (0.1% TFA) (0.025 g).

Aufarbeitung

  1. temperatureThe reaction mixture was cooled to room temperature
  2. filtrationfiltered
  3. custompurified by reverse phase HPLC
  4. washeluting with acetonitrile/water (0.1% TFA) (0.025 g)

Quellen und Nachweise

ORD-Eintrag
ord-e1f4ed265e034a7a8b4bb2f32b32ba0d
Quelldatensatz
uspto-grants-2010_05
Patentnummer
US07709503B2

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