反应 #343602

反应方程式

sodium nitrite

sodium nitrite

Ethyl propionylacetate

acetic acid

→

ethyl 2-propionyl-2-hydroxyiminoacetate

收率 69.4%

溶剂

water

反应条件

后处理

1. 1
   workup.ADDITIONwas added to the solution
2. 2
   workup.STIRRINGstirred at 25° C. for 1.5 hrs
3. 3
   workup.STIRRINGstirred at room temperature for 2 hrs
4. 4
   萃取The reaction mixture was extracted with diethyl ether (50 ml.) twice
5. 5
   洗涤the extract was washed with saturated aqueous sodium bicarbonate (30 ml.) three times and saturated aqueous sodium chloride
6. 6
   干燥dried over magnesium sulfate
7. 7
   过滤filtered
8. 8
   其他The filtrate was evaporated in vacuo

实验过程

Ethyl propionylacetate (14.4 g.) was added to acetic acid (19 ml.) and stirred at 5° to 10° C. To the solution was added dropwise over 40 minutes about 2/3 volume of an aqueous solution (30 ml.) of sodium nitrite (15 g.), and further water (50 ml.) was added to the solution and stirred at 25° C. for 1.5 hrs. The remaining aqueous solution of sodium nitrite was added dropwise over 10 minutes to the solution and stirred at room temperature for 2 hrs. The reaction mixture was extracted with diethyl ether (50 ml.) twice, and the extract was washed with saturated aqueous sodium bicarbonate (30 ml.) three times and saturated aqueous sodium chloride, dried over magnesium sulfate and filtered. The filtrate was evaporated in vacuo to give ethyl 2-propionyl-2-hydroxyiminoacetate (12 g.).

来源