Cyanoacetic acid → HCID 53797226, 화합물

HRID 439568

반응식

HRID 439568 반응식
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[C:6]([O:12][CH3:13])[CH:5]=1)=O.[C:14]([CH2:16][C:17]([OH:19])=[O:18])#[N:15].C([O-])(=O)C.[NH4+].[OH-].[Na+]>C1C=CC=CC=1.O.C(Cl)(Cl)Cl.C(O)(=O)C>[C:14]([CH:16]([CH:2]([CH3:1])[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[C:6]([O:12][CH3:13])[CH:5]=1)[C:17]([OH:19])=[O:18])#[N:15]

참가 물질

9

반응물 4

HCID 9740Cyanoacetic acidHCID 143283,4-Dimethoxyphenyl methyl ketoneHCID 14798Sodium HydroxideHCID 517165Ammonium Acetate2회

생성물 1

HCID 53797226HCID 53797226, 화합물수율 29%

시약·촉매·용매 4

HCID 176Acetic Acid용매HCID 241Benzene용매HCID 962Water용매HCID 6212Chloroform용매

실험 절차

To a solution of 3, 4-dimethoxyacetophenone (5.68 g, 31.53 mmol) and cyanoacetic acid (2.95 g, 34.68 mmol) in benzene were added acetic acid (1.9 ml) and ammonium acetate (150 mg), and the resultant mixture was refluxed with Dean Stark's dehydrating apparatus for 13 hours while adding ammonium acetate (130 mg) every 4 hours. The mixture was mixed with chloroform (200 ml), 2N aqueous sodium hydroxide solution (100 ml) and water (200 ml), stirred well and the aqueous layer was separated. The aqueous layer was acidified with dilute hydrochloric acid, and the resulting precipitate was filtered off. The residue was washed with diethyl ether to give a carboxylic acid, 2-cyano-3-methyl-3-(3, 4-dimethoxyphenyl) propionic acid (2.25 g, 29%).

후처리

  1. customfor 13 hours
  2. customthe aqueous layer was separated
  3. filtrationthe resulting precipitate was filtered off
  4. washThe residue was washed with diethyl ether

출처 및 근거

ORD 기록
ord-f0b4f5986f8848e384f73298b1fa4404
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05514711

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