O-Methylhydroxylamine → 1-Methoxy-3-(1,2,3,4-tetrahydro-4-oxo-1-naphthyl)urea

HRID 1730726Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1730726
[CH3:1][O:2][NH2:3].C(N(CC)CC)C.[O:11]=[C:12]1[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH:15]([N:22]=[C:23]=[O:24])[CH2:14][CH2:13]1>C(Cl)Cl>[CH3:1][O:2][NH:3][C:23]([NH:22][CH:15]1[C:16]2[C:21](=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:12](=[O:11])[CH2:13][CH2:14]1)=[O:24]

Komponenten

5

Edukt 3

HCID 4113O-MethylhydroxylamineHCID 8471TriethylamineHCID 203516844-Isocyanato-3,4-dihydronaphthalen-1(2H)-one

Produkt 1

HCID 203516951-Methoxy-3-(1,2,3,4-tetrahydro-4-oxo-1-naphthyl)urea

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

A mixture of N-methoxyamine (2.5 g), triethylamine (3.04 g) and dry methylene chloride (50 ml) is stirred at room temperature for 20 minutes under a nitrogen atmosphere. Then a solution of 1,2,3,4-tetrahydro-4-oxo-1-naphthyl isocyanate (5.62 g) in dry methylene chloride (50 ml) is added dropwise. After stirring at room temperature for 40 minutes, the reaction mixture is evaporated to dryness in vacuo and the solid residue washed with water (3 × 150 ml) to yield 6.1 g. title product, m.p. 148° to 151° C. Recrystallization from benzene affords crystals, m.p. 155° to 158° C.

Aufarbeitung

  1. stirringAfter stirring at room temperature for 40 minutes
  2. customthe reaction mixture is evaporated to dryness in vacuo
  3. washthe solid residue washed with water (3 × 150 ml)
  4. customto yield 6.1 g

Quellen und Nachweise

ORD-Eintrag
ord-c897f0c38b0f4aecaa7953b7178bd282
Quelldatensatz
uspto-grants-1976_11
Patentnummer
US03993677

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