Water → (3,6-Dichloropyridazin-4-yl)diethylamine

HRID 217704

Reaktionsgleichung

Reaktionsgleichung von HRID 217704
[Cl:1][C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1Cl.[CH2:10]([NH:12][CH2:13][CH3:14])[CH3:11].O.CC(=O)OCC>C1(C)C=CC=CC=1>[Cl:1][C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1[N:12]([CH2:13][CH3:14])[CH2:10][CH3:11]

Komponenten

6

Versuchsvorschrift

3,4,6-Trichloropyridazine (2 g) and diethylamine (2.4 ml) were initially charged in toluene (10 ml) and left to stand at RT for 3 days. Then the mixture was admixed with water and EA, and the EA phase was removed. The EA phase was washed three times with water, dried over magnesium sulfate, filtered and concentrated. The residue was purified using silica gel (70 g cartridge, n-heptane/EA gradient 0-50% within 60 min). 1.1 g of the title compound were obtained.

Aufarbeitung

  1. waitleft
  2. customthe EA phase was removed
  3. washThe EA phase was washed three times with water
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue was purified
  8. customsilica gel (70 g cartridge, n-heptane/EA gradient 0-50% within 60 min)

Quellen und Nachweise

ORD-Eintrag
ord-8b427b2e1e5a481394b1b715a71e768f
Quelldatensatz
uspto-grants-2012_06
Patentnummer
US08198272B2

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