Urea → 3,3-Dimethyl-2,6-piperidinedione

HRID 1008737

反応式

HRID 1008737 の反応式
[CH3:1][C:2]([CH3:11])([CH2:6][CH2:7][C:8](O)=[O:9])[C:3](O)=[O:4].[NH2:12]C(N)=O>O>[CH3:1][C:2]1([CH3:11])[CH2:6][CH2:7][C:8](=[O:9])[NH:12][C:3]1=[O:4]

参加物

4

反応物 2

HCID 1176UreaHCID 126812,2-Dimethylglutaric acid

生成物 1

HCID 1210483,3-Dimethyl-2,6-piperidinedione収率 86.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
160 °C

実験手順

The mixture of 10 g of 2,2-dimethylglutaric acid and 37.5 g of urea was stirred for 8 hours at 160° C. Into the reaction mixture was added water at 100° C., and the mixture was cooled to near room temperature. The mixture was extracted with ethyl acetate three times. The organic layers were washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 7.6 g of 3,3-dimethylpiperidin-2,6-dione.

後処理

  1. temperaturethe mixture was cooled to near room temperature
  2. extractionThe mixture was extracted with ethyl acetate three times
  3. washThe organic layers were washed with a saturated sodium chloride aqueous solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-3c46b5a6c0dc4f8fbcbdb201366827e0
出典データセット
uspto-grants-2011_07
特許番号
US07973028B2

関連ノート

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