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Sodium Hydroxide → 3-[N-(2,2,5,5-Tetramethyl-1,3-dioxane-4-carbonyl)amino]propionic acid

HRID 892874
ノート
印刷プレビュー

反応式

HRID 892874 の反応式
[OH-].[Na+].[CH3:3][C:4]1([CH3:27])[O:9][CH:8]([C:10]([NH:12][CH2:13][CH2:14][C:15]([O:17]CC2C=CC=CC=2)=[O:16])=[O:11])[C:7]([CH3:26])([CH3:25])[CH2:6][O:5]1>CO>[CH3:3][C:4]1([CH3:27])[O:9][CH:8]([C:10]([NH:12][CH2:13][CH2:14][C:15]([OH:17])=[O:16])=[O:11])[C:7]([CH3:26])([CH3:25])[CH2:6][O:5]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 19893743benzyl 3-[N-(2,2,5,5-Tetramethyl-1,3-dioxane-4-carbonyl)amino]propionate

生成物 1

HCID 189385173-[N-(2,2,5,5-Tetramethyl-1,3-dioxane-4-carbonyl)amino]propionic acid収率 78.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

An aqueous 1N sodium hydroxide solution (100 ml) was added to a solution 35 g of benzyl 3-[N-(2,2,5,5-Tetramethyl-1,3-dioxane-4-carbonyl)amino]propionate in 350 ml of methanol, and the mixture was stirred under ice cooling for 1 hour. After completion of the reaction, methanol was distilled off under reduced pressure. The aqueous layer was extracted with ethyl acetate. After adding 1N hydrochloric acid to the aqueous layer to render it acidic, the aqueous layer was extracted with ethyl acetate. The organic layer washed with water and then with saturated saline, and dried over anhydrous sodium sulfate. Removal of the solvent by evapoation afforded 20.4 g of the objective compound (yield: 78%).

後処理

  1. distillationwas distilled off under reduced pressure
  2. extractionThe aqueous layer was extracted with ethyl acetate
  3. additionAfter adding 1N hydrochloric acid to the aqueous layer
  4. extractionthe aqueous layer was extracted with ethyl acetate
  5. washThe organic layer washed with water
  6. dry with materialwith saturated saline, and dried over anhydrous sodium sulfate
  7. customRemoval of the solvent by evapoation

出典と根拠

ORDレコード
ord-83bd17a0a4814da8ab297587e8654464
出典データセット
uspto-grants-1992_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05120738

反応ノート

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