Reaktion #156133

Reaktionsgleichung

1-ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepine-7-carbaldehyde

2-methyl-2-butene

sodium dihydrogenphosphate

sodium chlorite

→

title compound

Ausbeute 44.0%

1-Ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepine-7-carboxylic acid

Ausbeute 44.0%

Lösungsmittel

H2O

t-butanol

Water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionfollowed by extraction
2. 2
   TrocknenThe organic layer was dried with sodium sulfate
3. 3
   Sonstigecondensed under reduced pressure

Vorschrift

To a t-butanol (20 ml) and H2O (5 ml) solution of 1-ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepine-7-carbaldehyde (2.25 g) and 2-methyl-2-butene (3.25 ml) were added sodium dihydrogenphosphate (0.92 g) and sodium chlorite (2.081 g), and the mixture was stirred at room temperature overnight. Water was added to the reaction mixture, followed by extraction using ethyl acetate. The organic layer was dried with sodium sulfate, and was condensed under reduced pressure to give the title compound (0.98 g) as a white powder.

Quelle