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Propanoic acid, 2-bromo-2-methyl-, ethyl ester → HCID 20329874, 화합물

HRID 2058083
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HRID 2058083 반응식
[Na].[C:2]1([CH3:17])[CH:7]=[CH:6][C:5]([N:8]=[CH:9][C:10]2[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=2)=[CH:4][CH:3]=1.Br[C:19]([CH3:26])([CH3:25])[C:20]([O:22][CH2:23][CH3:24])=[O:21]>C(O)C>[C:2]1([CH3:17])[CH:3]=[CH:4][C:5]([N:8]=[CH:9][C:10]2[CH:15]=[CH:14][C:13]([O:16][C:19]([CH3:26])([CH3:25])[C:20]([O:22][CH2:23][CH3:24])=[O:21])=[CH:12][CH:11]=2)=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11745Propanoic acid, 2-bromo-2-methyl-, ethyl esterHCID 6111664-{(E)-[(4-methylphenyl)imino]methyl}phenolHCID 5360545Sodium

생성물 1

HCID 20329874HCID 20329874, 화합물수율 61.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

(a) To 50 ml of absolute ethanol is added 0.58 g of sodium, and 4.2 g of 4-[N-(p-tolyl)formimidoyl]phenol and then 7.84 g of ethyl 2-bromo-2-methylpropionate are added to the solution at room temperature with stirring. The mixture is refluxed under heating and with stirring for 5 hours on an oil bath. After distilling off the ethanol from the reaction mixture, the residue is dissolved in ether. The solution is washed with 5% aqueous solution of sodium hydroxide and then with water. After drying the solution, the ether is distilled off, and the residue is further concentrated under reduced pressure on an oil bath at 100° C. to give 4.0 g of ethyl 2-[4-{N-(p-tolyl)formimidoyl}phenoxy]-2-methylpropionate as an oily product.

후처리

  1. temperatureThe mixture is refluxed
  2. temperatureunder heating
  3. stirringwith stirring for 5 hours on an oil bath
  4. distillationAfter distilling off the ethanol from the reaction mixture
  5. dissolutionthe residue is dissolved in ether
  6. washThe solution is washed with 5% aqueous solution of sodium hydroxide
  7. customAfter drying the solution
  8. distillationthe ether is distilled off
  9. concentrationthe residue is further concentrated under reduced pressure on an oil bath at 100° C.

출처 및 근거

ORD 기록
ord-67ed7e337b5847bba5f361e2a1d148d5
출처 데이터셋
uspto-grants-1980_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04214094

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