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

HRID 892874
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HRID 892874 반응식
[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
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참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-83bd17a0a4814da8ab297587e8654464
출처 데이터셋
uspto-grants-1992_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05120738

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