Water → HCID 22033802, Verbindung

HRID 2163519Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2163519
[C:1]([CH2:4][C:5](=[O:7])[CH3:6])(=[O:3])[CH3:2].C(N(CC)CC)C.[C:15]1([N:21]=[C:22]=[O:23])[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.O>C1C=CC=CC=1>[C:1]([CH:4]([C:5](=[O:7])[CH3:6])[C:22]([NH:21][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[O:23])(=[O:3])[CH3:2]

Komponenten

6

Edukt 4

HCID 962WaterHCID 7672Phenyl isocyanateHCID 8471TriethylamineHCID 31261Acetylacetone

Produkt 1

HCID 22033802HCID 22033802, VerbindungAusbeute 73 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel2×

Versuchsvorschrift

A mixture of acetylacetone (5 g) and triethylamine (5.2 g) in dry benzene (50 ml) was treated with phenyl isocyanate (6 g) in dry benzene (25 ml). The mixture was stirred for 3 hr at room temperature. Water (50 ml) was then added, the mixture shaken and the water layer separated. The benzene solution was extracted with two further portions (25 ml) of water and the combined aqueous extracts acidified with dilute hydrochloric acid. The product precipitated and was collected by filtration, washed with water and dried. Diacetyl acetanilide (7.0 g, 73%) was obtained as a colourless solid, m.p. 119-121° C.

Aufarbeitung

  1. stirringthe mixture shaken
  2. customthe water layer separated
  3. extractionThe benzene solution was extracted with two further portions (25 ml) of water
  4. customThe product precipitated
  5. filtrationwas collected by filtration
  6. washwashed with water
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-f461f0e1bcd84d2082fefe54d3d0ce03
Quelldatensatz
uspto-grants-1979_01
Patentnummer
US04134987

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