Sodium Hydroxide → 1-[8-(tert-butyl)-3,4-dihydro-2H-1,4-benzoxazin-6-yl]-1-ethanone

HRID 1295998Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1295998
[OH-].[Na+].C([N:6]1[C:11]2[CH:12]=[C:13]([C:20](=[O:22])[CH3:21])[CH:14]=[C:15]([C:16]([CH3:19])([CH3:18])[CH3:17])[C:10]=2[O:9][CH2:8][CH2:7]1)(=O)C>CO>[C:16]([C:15]1[C:10]2[O:9][CH2:8][CH2:7][NH:6][C:11]=2[CH:12]=[C:13]([C:20](=[O:22])[CH3:21])[CH:14]=1)([CH3:19])([CH3:17])[CH3:18]

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 589100091-[4-Acetyl-8-(tert-butyl)-3,4-dihydro-2H-1,4-benzoxazin-6-yl]-1-ethanone

Produkt 1

HCID 589099341-[8-(tert-butyl)-3,4-dihydro-2H-1,4-benzoxazin-6-yl]-1-ethanoneAusbeute 98,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

After adding 6 N aqueous sodium hydroxide (180 ml, 900 mmol) to a solution of the 1-[4-acetyl-8-(tert-butyl)-3,4-dihydro-2H-1,4-benzoxazin-6-yl]-1-ethanone (36.8 g, 134 mmol) in methanol (360 ml) under a nitrogen atmosphere, the mixture was stirred at 70° C. for 40 minutes. The methanol was distilled off under reduced pressure, and the precipitated crystals were filtered out and dried under reduced pressure to yield the title compound (30.6 g, 98.1% yield) as bright golden yellow crystals.

Aufarbeitung

  1. distillationThe methanol was distilled off under reduced pressure
  2. filtrationthe precipitated crystals were filtered out
  3. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-a1994b38a0ae46abab09b03c403154e4
Quelldatensatz
uspto-grants-2007_07
Patentnummer
US07244730B2

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