Hydrochloric Acid → 4-(2',4'-Dichlorophenoxy)-alpha-phenoxy-propionic acid isopropyl ester

HRID 1074514노트

반응식

HRID 1074514 반응식
[Cl:1][C:2]1[CH:20]=[C:19]([Cl:21])[CH:18]=[CH:17][C:3]=1[O:4][C:5]1[CH:16]=[CH:15][C:8]([O:9][CH:10]([CH3:14])[C:11]([OH:13])=[O:12])=[CH:7][CH:6]=1.Cl.[CH:23](O)([CH3:25])[CH3:24]>>[CH:23]([O:12][C:11](=[O:13])[CH:10]([O:9][C:8]1[CH:15]=[CH:16][C:5]([O:4][C:3]2[CH:17]=[CH:18][C:19]([Cl:21])=[CH:20][C:2]=2[Cl:1])=[CH:6][CH:7]=1)[CH3:14])([CH3:25])[CH3:24]

참가 물질

4

반응물 3

HCID 313Hydrochloric Acid2회HCID 3776IsopropanolHCID 386872-(4-(2,4-Dichlorophenoxy)phenoxy)propionic acid

생성물 1

HCID 127677994-(2',4'-Dichlorophenoxy)-alpha-phenoxy-propionic acid isopropyl ester

실험 절차

55 g of 4-(2',4'-dichlorophenoxy)-α-phenoxy-propionic acid were suspended in 500 ml of isopropanol. While stirring, hydrogen chloride was fed in, whereupon the temperature rose to about 50° C. While the feed of hydrogen chloride was continued, the suspension was refluxed for 5 hours and the reaction mixture was then allowed to stand overnight. After the excess alcohol had been distilled off, the solution was poured on water and then extracted with methylene chloride. The methylene chloride extract was washed with dilute bicarbonte solution and then twice with water and dried over sodium sulfate. After filtration the solution was concentrated and then distilled under greatly reduced pressure. 34 g of 4-(2',4'-dichlorophenoxy)-α-phenoxy-propionic acid isopropyl ester were obtained, boiling point 182°-185° C. under a pressure of 0.04 mm mercury.

후처리

  1. customrose to about 50° C
  2. temperaturethe suspension was refluxed for 5 hours
  3. distillationAfter the excess alcohol had been distilled off
  4. additionthe solution was poured on water
  5. extractionextracted with methylene chloride
  6. extractionThe methylene chloride extract
  7. washwas washed
  8. additionwith dilute bicarbonte solution
  9. dry with materialtwice with water and dried over sodium sulfate
  10. filtrationAfter filtration the solution
  11. concentrationwas concentrated
  12. distillationdistilled under greatly reduced pressure

출처 및 근거

ORD 기록
ord-5058ae70f2dc4e6295be66bb3b3d5ce9
출처 데이터셋
uspto-grants-1983_07
특허 번호
US04391995

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