Bromine → HCID 21837347, Verbindung

HRID 725277Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 725277
[Br:1]Br.[CH2:3]([C:5]1[CH:9]=[C:8]([CH2:10][CH3:11])[N:7]([C:12]2[C:17]([CH3:18])=[CH:16][C:15]([CH3:19])=[CH:14][C:13]=2[CH3:20])[N:6]=1)[CH3:4]>C(O)(=O)C>[Br:1][C:9]1[C:5]([CH2:3][CH3:4])=[N:6][N:7]([C:12]2[C:17]([CH3:18])=[CH:16][C:15]([CH3:19])=[CH:14][C:13]=2[CH3:20])[C:8]=1[CH2:10][CH3:11]

Komponenten

4

Edukt 2

HCID 24408BromineHCID 218373383,5-Diethyl-1-(2,4,6-trimethylphenyl)-1H-pyrazole

Produkt 1

HCID 21837347HCID 21837347, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel2×

Versuchsvorschrift

A solution of 6.4 g (0.04 mol) of bromine in 20 mL of glacial acetic acid was added dropwise to a stirred solution of 9.00 g (37 mmol) of 3,5-diethyl-1-(2,4,6-trimethylphenyl)pyrazole in 100 mL of glacial acetic acid. After 1 hour at room temperature, the acetic acid was evaporated under reduced pressure and the residues were dissolved in ethyl acetate. This solution was washed with saturated sodium bicarbonate to remove residual acetic acid, dried with brine and magnesium sulfate, and was concentrated on the rotovap. The product was a tan solid (10.26 g, purification. 1H-NMR(CDCl3):0.92 (3H, t, J=7), 1.15 (3H, t, J=7), 1.86 (6H, s), 2.24 (3H, s), 2.32 (2H, q, J=7), 2.60 (2H, q, J=7), 6.82 (2H, s).

Aufarbeitung

  1. customthe acetic acid was evaporated under reduced pressure
  2. dissolutionthe residues were dissolved in ethyl acetate
  3. washThis solution was washed with saturated sodium bicarbonate
  4. customto remove residual acetic acid
  5. dry with materialdried with brine and magnesium sulfate
  6. concentrationwas concentrated on the rotovap
  7. custom10.26 g, purification

Quellen und Nachweise

ORD-Eintrag
ord-5b268863696546f9aebf52fa3e9a5e27
Quelldatensatz
uspto-grants-1998_01
Patentnummer
US05705646

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