Реакция #217448

Уравнение реакции

ethyl acetoacetate

piperidine

stearylamine

ethyl cyanoacetate

hydrochloric acid

→

beige powder

Выход 65.7%

Stearyl Pyridone

Выход 65.7%

Растворители

dimethylformamide

methanol

Условия реакции

Обработка

1. 1
   ДругоеInto a 2 liter Erlenmeyer flask equipped
2. 2
   ТемператураThe mixture was heated to 120° C. for 4 hours
3. 3
   Температураto cool to room temperature
4. 4
   workup.STIRRINGto stir for 10 minutes
5. 5
   Фильтрацияwas then filtered
6. 6
   Промывкаwashed with 3×200 milliliter portions of methanol
7. 7
   Другоеdried at 60° C.

Методика

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.

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