反应 #710526

反应方程式

Compound I

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

NH2OH

pyridine

→

Compound J

收率 96.0%

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

收率 96.0%

溶剂

ethanol

HCl

反应条件

后处理

1. 1
   其他The reaction mixture was evaporated to dryness
2. 2
   workup.ADDITIONadded 10 mL of ethyl acetate
3. 3
   洗涤The organic layer was washed with distilled water
4. 4
   干燥dried over anhydrous sodium sulfate
5. 5
   过滤filtered
6. 6
   其他evaporated
7. 7
   其他The crude reaction mixture
8. 8
   其他was purified over silica gel column

实验过程

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.

来源