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Acetic Acid → HCID 13066676, 화합물

HRID 1163988
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HRID 1163988 반응식
[CH3:1][O:2][C:3]1[C:8]([O:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[CH3:16])=[CH:7][CH:6]=[CH:5][C:4]=1CC#N.Cl.[C:21]([OH:24])(=[O:23])[CH3:22]>>[CH3:1][O:2][C:3]1[C:8]([O:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[CH3:16])=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:22][C:21]([OH:24])=[O:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 20513415HCID 20513415, 화합물

생성물 1

HCID 13066676HCID 13066676, 화합물

실험 절차

2-[2-Methoxy-3-(o-tolyloxy)phenyl]acetonitrile (43.0 g) was added to a mixture of acetic acid (200 ml) and conc. hydrochloric acid (50 ml), and the mixture ws refluxed under heating for 5 hrs. The reaction mixture was evaporated, and water was added to the residue and extracted with diethyl ether. The extract was washed with water and extracted with aqueous sodium bicarbonate. The aqueous extract was washed with diethyl ether, acidified with conc. hydrochloric acid and then extracted with diethyl ether. The ether extract was dried over magnesium sulfate and evaporated. The crystalline residue (37.50 g) was recrystallized from a mixture of diisopropyl ether and n-hexane to give 2-[2-methoxy-3-(o-tolyloxy)phenyl]acetic acid (34.5 g). mp 90°-92° C.

후처리

  1. temperaturethe mixture ws refluxed
  2. temperatureunder heating for 5 hrs
  3. customThe reaction mixture was evaporated
  4. additionwater was added to the residue
  5. extractionextracted with diethyl ether
  6. washThe extract was washed with water
  7. extractionextracted with aqueous sodium bicarbonate
  8. extractionThe aqueous extract
  9. washwas washed with diethyl ether
  10. extractionextracted with diethyl ether
  11. extractionThe ether extract
  12. dry with materialwas dried over magnesium sulfate
  13. customevaporated
  14. customThe crystalline residue (37.50 g) was recrystallized from a mixture of diisopropyl ether and n-hexane

출처 및 근거

ORD 기록
ord-de82f9b4445b4e619b205e65c3c3287a
출처 데이터셋
uspto-grants-1983_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04367238

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