Reaktion #710526

Reaktionsgleichung

Compound I

2-(1,3-benzodioxol-5-yl)-2-methyl propanal

NH2OH

pyridine

→

Compound J

Ausbeute 96.0%

2-(1,3-benzodioxol-5-yl)-2-methyl propanal oxime

Ausbeute 96.0%

Lösungsmittel

ethanol

HCl

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe reaction mixture was evaporated to dryness
2. 2
   workup.ADDITIONadded 10 mL of ethyl acetate
3. 3
   WaschenThe organic layer was washed with distilled water
4. 4
   Trocknendried over anhydrous sodium sulfate
5. 5
   Filtrationfiltered
6. 6
   Sonstigeevaporated
7. 7
   SonstigeThe crude reaction mixture
8. 8
   Sonstigewas purified over silica gel column

Vorschrift

To a solution of Compound I (511 mg, 2.66 mmol) in ethanol (1 mL), HCl.NH2OH (277 mg, 4.00 mmol) and pyridine (2.2 mL, 26.58 mmol) were added and it was stirred at room temperature for 1.5 hours. The reaction mixture was evaporated to dryness and added 10 mL of ethyl acetate. The organic layer was washed with distilled water, dried over anhydrous sodium sulfate, filtered and evaporated. The crude reaction mixture was purified over silica gel column using 5:1 petroleum ether-ethyl acetate as solvent to afford Compound J (528 mg, 96%) as a white foam.

Quelle