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Sodium Hydroxide → 2-(2-(tert-Butyl)pyrimidin-5-yl)-3-methylbut-2-enoic acid

HRID 1085712
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HRID 1085712 반응식
[OH-].[Na+].[CH3:3][C:4]([C:7]1[N:12]=[CH:11][C:10]([C:13](=[C:19]([CH3:21])[CH3:20])[C:14]([O:16]CC)=[O:15])=[CH:9][N:8]=1)([CH3:6])[CH3:5]>C(O)(C)C.O>[CH3:6][C:4]([C:7]1[N:8]=[CH:9][C:10]([C:13](=[C:19]([CH3:21])[CH3:20])[C:14]([OH:16])=[O:15])=[CH:11][N:12]=1)([CH3:3])[CH3:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 14718883HCID 14718883, 화합물

생성물 1

HCID 147188842-(2-(tert-Butyl)pyrimidin-5-yl)-3-methylbut-2-enoic acid

시약·촉매·용매 2

HCID 962Water용매HCID 3776Isopropanol용매

실험 절차

A solution of sodium hydroxide 0.24 g) and ethyl 2-[2-(1,1-dimethylethyl)pyrimidin-5-yl]-3-methylbut-2-enoate (0.4 g) in isopropanol (10 cm3) and water (2 cm3) was heated to the reflux temperature for a period of 3 hours. After cooling to the ambient temperature the crude reaction mixture was concentrated by evaporation of the solvent under reduced pressure, and the residue was dissolved in water, and extracted with ethyl acetate. The aqueous portion was acidified with dilute hydrochloric acid, and extracted with ethyl acetate. The combined organic extracts were washed with water, dried over anhydrous magnesium sulphate and concentrated by evaporation of the solvent under reduced pressure to give 2-[2-(1,1-dimethylethyl)pyrimidin-5-yl]-3-methylbut-2-enoic acid, containing a small amount of 2-[2-(1,1-dimethylethyl)pyrimidin-5-yl]-3-methylbut-3-enoic acid. The crude produce was used without further purification.

후처리

  1. customreaction mixture
  2. concentrationwas concentrated by evaporation of the solvent under reduced pressure
  3. dissolutionthe residue was dissolved in water
  4. extractionextracted with ethyl acetate
  5. extractionextracted with ethyl acetate
  6. washThe combined organic extracts were washed with water
  7. dry with materialdried over anhydrous magnesium sulphate
  8. concentrationconcentrated by evaporation of the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-c76db4a086e54ba7b0f530a7b14017ef
출처 데이터셋
uspto-grants-1991_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05010200

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