Acetic Acid → 3-Methyl-2,6-piperidinedione

HRID 75946

反応式

HRID 75946 の反応式
OS(O)(=O)=O.[C:6]([OH:9])(=O)[CH3:7].[CH3:10][CH:11]([CH2:14]CC#N)[C:12]#[N:13].C([O-])([O-])=[O:19].[Na+].[Na+]>O>[CH3:10][CH:11]1[CH2:14][CH2:7][C:6](=[O:9])[NH:13][C:12]1=[O:19]

参加物

6

反応物 4

HCID 176Acetic Acid2 回HCID 1118Sulfuric AcidHCID 10340Sodium CarbonateHCID 206862-Methylpentanedinitrile

生成物 1

HCID 346293-Methyl-2,6-piperidinedione収率 67%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
130 °C

実験手順

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.

後処理

  1. additionUpon completion of the addition
  2. temperatureto cool to room temperature
  3. filtrationfiltered
  4. customto remove solids, which
  5. washwere washed with acetic acid (100 ml)
  6. concentrationThe filtrate was then concentrated until a residue
  7. customresulted
  8. filtrationThe resulting solid was collected by filtration
  9. washwashed with cold water

出典と根拠

ORDレコード
ord-faca0af8e1974591a4fb020f2178728c
出典データセット
uspto-grants-2014_09
特許番号
US08835465B2

関連ノート

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