تفاعل #7311

معادلة التفاعل

5-acetoxy-4-methyl-3,4-dihydro-2H-pyridine-1-carboxylic acid methyl ester

water

sodium carbonate

sodium bicarbonate

→

4-Methyl-3-oxo-piperidine-1-carboxylic acid methyl ester

المردود 32.0%

المذيبات

Methanol

methanol

methanol

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGstirred at room temperature for 18 hours
2. 2
   تركيزThe mixture was then concentrated
3. 3
   أخرىto remove methanol
4. 4
   workup.ADDITIONWater was added to the mixture
5. 5
   workup.DISSOLUTIONto dissolve all salts
6. 6
   استخلاصThis was then extracted with ethyl acetate three times
7. 7
   تجفيفdried over magnesium sulfate
8. 8
   ترشيحfiltered
9. 9
   أخرىevaporated

الإجراء التجريبي

In a 1000 ml round bottom flask, 50 g of crude 5-acetoxy-4-methyl-3,4-dihydro-2H-pyridine-1-carboxylic acid methyl ester was dissolved in 200 ml of methanol. To 300 ml water was added 30 g of sodium carbonate and 30 g sodium bicarbonate (pH=10). The aqueous buffer was added to the methanol solution. Methanol was added to the mixture until it stirred easily, and stirred at room temperature for 18 hours. The mixture was then concentrated to remove methanol. Water was added to the mixture to dissolve all salts. This was then extracted with ethyl acetate three times. The organic extracts were combined, dried over magnesium sulfate, filtered, and evaporated to furnish the crude compound 4-Methyl-3-oxo-piperidine-1-carboxylic acid methyl ester as oil, which was then purified as described below.

المصدر