Urea → 3,3,5,5-Tetramethylpiperidine-2,6-dione

HRID 2425934ノート

反応式

HRID 2425934 の反応式
[CH3:1][C:2]([CH3:13])([C:10](O)=[O:11])[CH2:3][C:4]([CH3:9])([CH3:8])[C:5](O)=[O:6].[NH2:14]C(N)=O>O>[CH3:1][C:2]1([CH3:13])[CH2:3][C:4]([CH3:9])([CH3:8])[C:5](=[O:6])[NH:14][C:10]1=[O:11]

参加物

4

反応物 2

HCID 1176UreaHCID 12290289Pentanedioic acid, 2,2,4,4-tetramethyl-

生成物 1

HCID 133786663,3,5,5-Tetramethylpiperidine-2,6-dione収率 98.4%

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 2.6 g of tetramethylglutaric acid and 8.3 g of urea was stirred for 10 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 2.3 g of 3,3,5,5-tetramethylpiperidin-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-84079ad4f1af4a00a57fd6e0a7f09d19
出典データセット
uspto-grants-2011_06
特許番号
US07968537B2

反応ノート

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