Nitrogen → HCID 66929097, Verbindung

HRID 2065076Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2065076
N#N.[N+:3]([C:6]1[CH:10]=[CH:9][N:8]([CH2:11][C:12]2[O:13][CH:14]=[C:15]([C:17](=[O:19])[CH3:18])[N:16]=2)[N:7]=1)([O-])=O.[NH4+].[Cl-]>CCO.O.[Fe]>[NH2:3][C:6]1[CH:10]=[CH:9][N:8]([CH2:11][C:12]2[O:13][CH:14]=[C:15]([C:17](=[O:19])[CH3:18])[N:16]=2)[N:7]=1

Komponenten

7

Edukt 3

HCID 947NitrogenHCID 25517Ammonium ChlorideHCID 669287371-[2-(3-Nitro-pyrazol-1-ylmethyl)-oxazol-4-yl]-ethanone

Produkt 1

HCID 66929097HCID 66929097, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 23925IronKatalysatorHCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
75 °C

Versuchsvorschrift

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of 1-[2-(3-nitro-pyrazol-1-ylmethyl)-oxazol-4-yl]-ethanone (48 mg, 0.20 mmol), iron powder (34 mg, 0.61 mmol) and NH4Cl (56 mg, 1.03 mmol) in a mixture of EtOH (2.0 mL) and water (1.0 mL) was stirred at 75° C. for 60 min. The reaction mixture was filtered while hot and concentrated under reduced pressure. CH2Cl2 (10 mL) was added followed by water (10 mL). The aq. layer was extracted with CH2Cl2 (2×10 mL) and the combined org. extracts were dried over Na2SO4, filtered, and the solvents were removed under reduced pressure to give the title compound as a yellow oil. TLC: rf (EA)=0.13. LC-MS-conditions 02: tR=0.38 min; [M+H]+=207.40.

Aufarbeitung

  1. filtrationThe reaction mixture was filtered while hot and
  2. concentrationconcentrated under reduced pressure
  3. additionCH2Cl2 (10 mL) was added
  4. extractionThe aq. layer was extracted with CH2Cl2 (2×10 mL)
  5. dry with materialextracts were dried over Na2SO4
  6. filtrationfiltered
  7. customthe solvents were removed under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-065d5d1b02a6444788ac01409187c053
Quelldatensatz
uspto-grants-2012_10
Patentnummer
US08288419B2

Notizen zur Reaktion

Wird geladen…