반응 #710526

반응 방정식

Compound I

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

NH2OH

pyridine

→

Compound J

수율 96.0%

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

수율 96.0%

용매

ethanol

HCl

반응 조건

후처리

1. 1
   기타The reaction mixture was evaporated to dryness
2. 2
   workup.ADDITIONadded 10 mL of ethyl acetate
3. 3
   세척The organic layer was washed with distilled water
4. 4
   건조dried over anhydrous sodium sulfate
5. 5
   여과filtered
6. 6
   기타evaporated
7. 7
   기타The crude reaction mixture
8. 8
   기타was purified over silica gel column

실험 절차

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.

출처