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Water → HCID 15007188, Verbindung

HRID 1085793
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1085793
[CH:1]([N:4]1[C:9](=[O:10])[C:8]([Br:11])=[C:7](Br)[CH:6]=[N:5]1)([CH3:3])[CH3:2].Cl.[CH3:14][O:15][C:16]1[CH:25]=[CH:24][C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[C:17]=1[CH2:26][NH2:27].C(=O)([O-])[O-].[Na+].[Na+].O>O1CCOCC1>[CH:1]([N:4]1[C:9](=[O:10])[C:8]([Br:11])=[C:7]([NH:27][CH2:26][C:17]2[C:18]3[C:23](=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH:24]=[CH:25][C:16]=2[O:15][CH3:14])[CH:6]=[N:5]1)([CH3:3])[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 10827742HCID 10827742, VerbindungHCID 20058940HCID 20058940, Verbindung

Produkt 1

HCID 15007188HCID 15007188, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-Dioxane
Lösungsmittel

Versuchsvorschrift

A mixture comprising 1.48 g of 2-i-propyl-4,5-dibromo-3(2H)pyridazinone, 1.68 g of 2-methoxy-1-naphthylmethylamine hydrochloride, 1.33 g of sodium carbonate, 30 ml of water and 30 ml of 1,4-dioxane, was refluxed under stirring overnight. Then, the solvent was distilled off under reduced pressure, and water was poured to the residue thus obtained. The mixture was extracted with ethyl acetate. The extract was washed sequentially with a 2 wt% hydrochloric acid aqueous solution, water and a saturated sodium chloride aqueous solution and then dried over sodium sulfate. Then, the solvent was distilled off. The residual solid thus obtained was crystallized from ethyl acetate/n-hexane to obtain 1.18 g of the above identified compound as colorless crystals having a melting point of from 160° to 161° C.

Aufarbeitung

  1. temperaturewas refluxed
  2. distillationThen, the solvent was distilled off under reduced pressure, and water
  3. additionwas poured to the residue
  4. customthus obtained
  5. extractionThe mixture was extracted with ethyl acetate
  6. washThe extract was washed sequentially with a 2 wt% hydrochloric acid aqueous solution, water
  7. dry with materiala saturated sodium chloride aqueous solution and then dried over sodium sulfate
  8. distillationThen, the solvent was distilled off
  9. customThe residual solid thus obtained
  10. customwas crystallized from ethyl acetate/n-hexane
  11. customto obtain 1.18 g of the
  12. customof from 160° to 161° C.

Quellen und Nachweise

ORD-Eintrag
ord-0fb402eda23a412b9a550654ed8594c9
Quelldatensatz
uspto-grants-1991_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05011839

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