反应 #2383807

反应方程式

2-nitroethanol

sodium acetate

acetic anhydride

2-nitroethanol

→

2-nitroethylacetate

溶剂

ethyl acetate

brine

反应条件

后处理

1. 1
   workup.STIRRINGthe orange reaction mixture was stirred at 0-5° C. for an additional hour
2. 2
   温度the exotherm of the reaction increased the temperature to 30° C.
3. 3
   温度the mixture was cooled with an ice bath to 20° C
4. 4
   workup.STIRRINGThe reaction was then stirred at ambient temperature under N2 overnight
5. 5
   其他The layers were separated
6. 6
   萃取the bottom aqueous layer was extracted again with ethyl acetate (25 mL)
7. 7
   洗涤The combined ethyl acetate layers were washed once with saturated brine (50 mL)
8. 8
   干燥dried (MgSO4)
9. 9
   过滤filtered
10. 10
    浓缩concentrated

实验过程

A mixture of sodium acetate (6.4 g, 78 mmol) and acetic anhydride (30 mL, 330 mmol) was stirred at 0-5° C. To this slurry was added 2-nitroethanol (30 g, 280 mmol) dropwise over a period of approximately 1 hour. After the 2-nitroethanol addition, the orange reaction mixture was stirred at 0-5° C. for an additional hour and then at ambient temperature for approximately 70 min, the exotherm of the reaction increased the temperature to 30° C. and the mixture was cooled with an ice bath to 20° C. The reaction was then stirred at ambient temperature under N2 overnight. The reaction mixture was diluted with ethyl acetate (EtOAc, 40 mL) and saturated brine (80 mL). The layers were separated and the bottom aqueous layer was extracted again with ethyl acetate (25 mL). The combined ethyl acetate layers were washed once with saturated brine (50 mL), dried (MgSO4), filtered and concentrated to afford 38 g of 2-nitroethylacetate as a reddish orange oil.

来源