2-Propanone, 1-(2-nitrophenoxy)- → 3-Methyl-3,4-dihydro-2H-1,4-benzoxazine

HRID 1515071

Reaktionsgleichung

Reaktionsgleichung von HRID 1515071
[H][H].[N+:3]([C:6]1[CH:16]=[CH:15][CH:14]=[CH:13][C:7]=1[O:8][CH2:9][C:10](=O)[CH3:11])([O-])=O.[N+](C(OC1C=CC=CC=1)C(=O)C)([O-])=O>[Ni].CO>[CH3:11][CH:10]1[NH:3][C:6]2[CH:16]=[CH:15][CH:14]=[CH:13][C:7]=2[O:8][CH2:9]1

Komponenten

6

Edukt 3

HCID 792392-Propanone, 1-(2-nitrophenoxy)-HCID 86645093Nitrophenoxyacetone2×HCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 27637603-Methyl-3,4-dihydro-2H-1,4-benzoxazine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 935NickelKatalysatorHCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

Reaction conditions: 220 bar of hydrogen, reaction temperature 60° C. with a residence time of about 60-90 minutes. The space velocity was about 2 g of o-nitrophenoxyacetone per g of catalyst used and hour. The catalyst used was a nickel sponge metal catalyst from H. C. Starck, Amperkat Ni—Mo 3706 (exchange of the water under which the catalyst is stored for methanol). The yields in this step were 95+%; at least 100 g of nitrophenoxyacetone were converted per gram of theoretically dry catalyst. Good mixing was ensured by stirring. In order to prevent precipitation of the reactant solution, it was heated to 40° C.

Aufarbeitung

  1. customReaction conditions
  2. waitused and hour
  3. customThe yields in this step
  4. additionGood mixing
  5. customprecipitation of the reactant solution, it

Quellen und Nachweise

ORD-Eintrag
ord-629711ecd6cc4ed6aa253eec72c81650
Quelldatensatz
uspto-grants-2012_07
Patentnummer
US08222408B2

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