Sodium Hydroxide → 2-{4-[(4-Chloroanilino)methyl]phenoxy}-2-methylpropanoic acid

HRID 2058089노트

반응식

HRID 2058089 반응식
[Cl:1][C:2]1[CH:24]=[CH:23][C:5]([NH:6][CH2:7][C:8]2[CH:22]=[CH:21][C:11]([O:12][C:13]([CH3:20])([CH3:19])[C:14]([O:16]CC)=[O:15])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[OH-].[Na+]>C(O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([NH:6][CH2:7][C:8]2[CH:9]=[CH:10][C:11]([O:12][C:13]([CH3:20])([CH3:19])[C:14]([OH:16])=[O:15])=[CH:21][CH:22]=2)=[CH:23][CH:24]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 20329838Ethyl 2-[4-(4-chloroanilinomethyl)phenoxy]-2-methylpropionate

생성물 1

HCID 203298652-{4-[(4-Chloroanilino)methyl]phenoxy}-2-methylpropanoic acid수율 99.2%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
70 °C

실험 절차

A mixture of 6.14 g of ethyl 2-[4-(4-chloroanilinomethyl)phenoxy]-2-methylpropionate, 130 ml of 95% ethanol and 52 ml of 1 N aqueous solution of sodium hydroxide is stirred at 70° C. for 50 minutes. After concentrating the reaction mixture under reduced pressure, the residue is dissolved in water and the solution is washed with ether five times. To the aqueous solution is added 55 ml of 1 N hydrochloric acid with cooling, and the precipitated crystals are extracted twice with ether. The extract is washed with water twice, then dried over magnesium sulfate and thereafter the solvent is distilled off to give 5.6 g of 2-[4-(4-chloroanilinomethyl)phenoxy]-2-methylpropionic acid, colorless crystals, mp 155° to 158° C.

후처리

  1. concentrationAfter concentrating the reaction mixture under reduced pressure
  2. dissolutionthe residue is dissolved in water
  3. washthe solution is washed with ether five times
  4. additionTo the aqueous solution is added 55 ml of 1 N hydrochloric acid
  5. temperaturewith cooling
  6. extractionthe precipitated crystals are extracted twice with ether
  7. washThe extract is washed with water twice
  8. dry with materialdried over magnesium sulfate
  9. distillationthe solvent is distilled off

출처 및 근거

ORD 기록
ord-c7b06c8273cf4097b4f0f90b13bf6e59
출처 데이터셋
uspto-grants-1980_07
특허 번호
US04214094

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