4-Methoxynaphthalen-1-ylmethylamine → 4-Chloro-5-(4-methoxy-1-naphthylmethylamino)-6-i-propoxy-3(2H)pyridazinone

HRID 1085796

Reaktionsgleichung

Reaktionsgleichung von HRID 1085796
[Cl:1][C:2]1[C:3](=[O:13])[NH:4][N:5]=[C:6]([O:9][CH2:10][CH2:11]C)[C:7]=1Cl.[CH3:14][O:15][C:16]1[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[C:19]([CH2:26][NH2:27])=[CH:18][CH:17]=1.O.O1CCOC[CH2:30]1>>[Cl:1][C:2]1[C:3](=[O:13])[NH:4][N:5]=[C:6]([O:9][CH:10]([CH3:11])[CH3:30])[C:7]=1[NH:27][CH2:26][C:19]1[C:20]2[C:25](=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:16]([O:15][CH3:14])=[CH:17][CH:18]=1

Komponenten

4

Edukt 3

HCID 591394-Methoxynaphthalen-1-ylmethylamineHCID 218864351,4-Dioxane--water (1/1)HCID 867447384,5 dichloro 6-1-propoxy-3(2H)pyridazinone

Produkt 1

HCID 150071934-Chloro-5-(4-methoxy-1-naphthylmethylamino)-6-i-propoxy-3(2H)pyridazinone

Versuchsvorschrift

A mixture comprising 350 mg of 4,5 dichloro 6-1-propoxy-3(2H)pyridazinone, 1.23 g of 4-methoxy-1-naphthylmethylamine and 30 ml of a mixture of water/1,4-dioxane (volume ratio of 1/1), was refluxed under stirring for 3.5 hours. The reaction mixture was concentrated, and precipitated crystals were collected by filtration and recrystallized from a mixture of methanol/water to obtain 420 mg of the above identified compound as colorless crystals having a melting point of from 244° to 247° C.

Aufarbeitung

  1. temperaturewas refluxed
  2. concentrationThe reaction mixture was concentrated
  3. customprecipitated crystals
  4. filtrationwere collected by filtration
  5. customrecrystallized from a mixture of methanol/water
  6. customto obtain 420 mg of the
  7. customof from 244° to 247° C.

Quellen und Nachweise

ORD-Eintrag
ord-bfdbea7e68c94d4d9fb2cdf137010c38
Quelldatensatz
uspto-grants-1991_04
Patentnummer
US05011839

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