反応 #217448

反応方程式

ethyl acetoacetate

piperidine

stearylamine

ethyl cyanoacetate

hydrochloric acid

→

beige powder

収率 65.7%

Stearyl Pyridone

収率 65.7%

溶媒

dimethylformamide

methanol

反応条件

後処理

1. 1
   その他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
   ろ過was then filtered
6. 6
   洗浄washed with 3×200 milliliter portions of methanol
7. 7
   その他dried at 60° C.

実験手順

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.

出典