Sodium Hydroxide → 2-(4-Nitrophenyl)propionic acid

HRID 2413908노트

반응식

HRID 2413908 반응식
[CH3:1][C:2]([C:13]1[CH:18]=[CH:17][C:16]([N+:19]([O-:21])=[O:20])=[CH:15][CH:14]=1)(C(OCC)=O)[C:3]([O:5]CC)=[O:4].[OH-].[Na+]>C(O)C.O>[N+:19]([C:16]1[CH:15]=[CH:14][C:13]([CH:2]([CH3:1])[C:3]([OH:5])=[O:4])=[CH:18][CH:17]=1)([O-:21])=[O:20]

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 12380744Diethyl methyl(4-nitrophenyl)propanedioate

생성물 1

HCID 892442-(4-Nitrophenyl)propionic acid수율 68.8%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

실험 절차

147 g of the crude diethyl 2-methyl-2-(4-nitrophenyl)-malonate was dissolved in 600 ml of ethanol, and to this was added a solution of 42.4 g (0.846 mole) of 93% sodium hydroxide in 400 ml of water and the solution was reacted at 50° C. for 3 hours. After that, to the reaction mixture was added 1 l of water and the formed oily substance and an aqueous layer were separated. The aqueous layer was acidified with conc. hydrochloric acid and was extracted with 700 ml of ethyl acetate. The ethyl acetate layer was washed with a saturated solution of sodium chloride and dried over anhydrous magnesium sulfate. After filtering out magnesium sulfate, ethyl acetate was distilled off to give 66.8 g of crude 2-(4-nitrophenyl)propionic acid.

후처리

  1. customthe solution was reacted at 50° C. for 3 hours
  2. customthe formed oily substance and an aqueous layer were separated
  3. extractionwas extracted with 700 ml of ethyl acetate
  4. washThe ethyl acetate layer was washed with a saturated solution of sodium chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationAfter filtering out magnesium sulfate, ethyl acetate
  7. distillationwas distilled off

출처 및 근거

ORD 기록
ord-ebc26e7989a84217bf46f5446e02ca5f
출처 데이터셋
uspto-grants-1988_01
특허 번호
US04720506

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