反应 #217448

反应方程式

ethyl acetoacetate

piperidine

stearylamine

ethyl cyanoacetate

hydrochloric acid

→

beige powder

收率 65.7%

Stearyl Pyridone

收率 65.7%

溶剂

dimethylformamide

methanol

反应条件

后处理

1. 1
   其他Into a 2 liter Erlenmeyer flask equipped
2. 2
   温度The mixture was heated to 120° C. for 4 hours
3. 3
   温度to cool to room temperature
4. 4
   workup.STIRRINGto stir for 10 minutes
5. 5
   过滤was then filtered
6. 6
   洗涤washed with 3×200 milliliter portions of methanol
7. 7
   其他dried at 60° C.

实验过程

Into a 2 liter Erlenmeyer flask equipped with magnetic stirring was charged stearylamine (118 g, 0.44 mol; obtained from Sigma-Aldrich) and ethyl cyanoacetate (ECA, 45.2 grams, 0.4 mol). The mixture was heated to 120° C. for 90 minutes, after which ethyl acetoacetate (EAA, 114 grams, 0.88 mol), piperidine (PIP; 70 grams, 0.82 mol), and dimethylformamide (DMF; 140 milliliters) were added. The mixture was heated to 120° C. for 4 hours. The mixture was then allowed to cool to room temperature and was poured slowly into well stirred methanol (1,200 milliliters), which contained concentrated hydrochloric acid (100 milliliters). The resulting suspension was allowed to stir for 10 minutes, and was then filtered and washed with 3×200 milliliter portions of methanol. The resulting solid was oven dried at 60° C. to give 91.3 grams of a beige powder at 57 percent yield.

来源