반응 #163128

반응 방정식

acetic acid

H2SO4

acetic acid

2-methylpentanedinitrile

Na2CO3

→

title compound

수율 67.0%

3-Methylpiperidine-2,6-dione

수율 67.0%

용매

water

반응 조건

후처리

1. 1
   workup.ADDITIONUpon completion of the addition
2. 2
   온도to cool to room temperature
3. 3
   여과filtered
4. 4
   기타to remove solids, which
5. 5
   세척were washed with acetic acid (100 ml)
6. 6
   농축The filtrate was then concentrated until a residue
7. 7
   기타resulted
8. 8
   여과The resulting solid was collected by filtration
9. 9
   세척washed with cold water

실험 절차

A solution of H2SO4 (80 ml), acetic acid (500 ml) and 2-methylpentanedinitrile (128.0 g, 1184 mmol) was stirred at room temperature. An aqueous solution of acetic acid (100 ml in 32 ml water) was then added dropwise. Upon completion of the addition, the reaction was heated to 130° C. for 1 hour. The reaction was then allowed to cool to room temperature and filtered to remove solids, which were washed with acetic acid (100 ml). The filtrate was then concentrated until a residue resulted. This residue was poured into water (0.75 l), and adjusted to pH 5 with Na2CO3. The resulting solid was collected by filtration and washed with cold water to give the title compound (101 g, 67%) which was used without further purification.

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