Water → 1-(2-Hydrazino-4-pyridyl)-3-hydroxymethyl-6,7-diethoxynaphthalene

HRID 324028

Reaktionsgleichung

Reaktionsgleichung von HRID 324028
Cl[C:2]1[CH:7]=[C:6]([C:8]2[C:17]3[C:12](=[CH:13][C:14]([O:21][CH2:22][CH3:23])=[C:15]([O:18][CH2:19][CH3:20])[CH:16]=3)[CH:11]=[C:10]([CH2:24][OH:25])[CH:9]=2)[CH:5]=[CH:4][N:3]=1.C(Cl)Cl.O.O.[NH2:31][NH2:32]>>[NH:31]([C:2]1[CH:7]=[C:6]([C:8]2[C:17]3[C:12](=[CH:13][C:14]([O:21][CH2:22][CH3:23])=[C:15]([O:18][CH2:19][CH3:20])[CH:16]=3)[CH:11]=[C:10]([CH2:24][OH:25])[CH:9]=2)[CH:5]=[CH:4][N:3]=1)[NH2:32]

Komponenten

5

Edukt 4

HCID 962WaterHCID 6344DichloromethaneHCID 24654Hydrazine hydrate (1:1)HCID 220073461-(2-Chloro-4-pyridyl)-3-hydroxymethyl-6,7-diethoxynaphthalene

Produkt 1

HCID 220073321-(2-Hydrazino-4-pyridyl)-3-hydroxymethyl-6,7-diethoxynaphthalene

Versuchsvorschrift

A suspension of 1-(2-chloro-4-pyridyl)-3-hydroxymethyl-6,7-diethoxynaphthalene (3.90 g) in hydrazine hydrate (17.8 ml) is refluxed for 9 hours. The mixture is stirred at room temperature for 10 minutes, and further stirred under ice-cooling for 10 minutes. To the mixture are added methylene chloride and water, and the methylene chloride layer is separated, washed, dried, and concentrated under reduced pressure to remove the solvent. The residue is dissolved in hot ethanol (20 ml), and allowed to cool overnight to give 1-(2-hydrazino-4-pyridyl)-3-hydroxymethyl-6,7-diethoxynaphthalene (3.19 g).

Aufarbeitung

  1. temperatureis refluxed for 9 hours
  2. stirringfurther stirred under ice-
  3. temperaturecooling for 10 minutes
  4. customthe methylene chloride layer is separated
  5. washwashed
  6. customdried
  7. concentrationconcentrated under reduced pressure
  8. customto remove the solvent
  9. dissolutionThe residue is dissolved in hot ethanol (20 ml)
  10. temperatureto cool overnight

Quellen und Nachweise

ORD-Eintrag
ord-9745631e4761464ebc95f8b0d92ca3ec
Quelldatensatz
uspto-grants-2001_04
Patentnummer
US06214996B1

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