3-Amino-6-chloro-4,5-dimethylpyridazine → HCID 71742687, Verbindung

HRID 1501344Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1501344
Cl[C:2]1[N:7]=[N:6][C:5]([NH2:8])=[C:4]([CH3:9])[C:3]=1[CH3:10].[CH3:11][O-:12].[Na+]>CO>[CH3:11][O:12][C:2]1[N:7]=[N:6][C:5]([NH2:8])=[C:4]([CH3:9])[C:3]=1[CH3:10]

Komponenten

4

Edukt 2

HCID 69919433-Amino-6-chloro-4,5-dimethylpyridazineHCID 10942334Sodium Methoxide

Produkt 1

HCID 71742687HCID 71742687, VerbindungAusbeute 49 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

6-Chloro-4,5-dimethylpyridazin-3-amine (CAS-Nr. 76593-36-7, 500 mg, 3.17 mmol, 1.0 eq) in 14.51 mL of a 25% solution (w/w) of sodium methylate in MeOH was heated for 1 h at 130° C. in a single mode microwave oven. The reaction mixture was partitioned between DCM and water. The organic phase was washed with brine and dried (Na2SO4 anh.). Volatile components were removed by the use of a rotary evaporator and the crude mixture was purified via MPLC (Biotage Isolera; 25 g SNAP NH2 cartridge: hexane→hexane/EtOAc 1/1) to give 250 mg (49% yield) of the title compound.

Aufarbeitung

  1. customThe reaction mixture was partitioned between DCM and water
  2. washThe organic phase was washed with brine
  3. dry with materialdried (Na2SO4 anh.)
  4. customVolatile components were removed by the use of a rotary evaporator
  5. customthe crude mixture was purified via MPLC (Biotage Isolera; 25 g SNAP NH2 cartridge: hexane→hexane/EtOAc 1/1)

Quellen und Nachweise

ORD-Eintrag
ord-e7bbc7c500d74f3ea9258285f2c94795
Quelldatensatz
uspto-grants-2015_12
Patentnummer
US09206185B2

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