Hydrochloric Acid → 4-{2,6-Dichloro-4-[(3,3-dichloroprop-2-EN-1-YL)oxy]phenoxy}butan-1-OL

HRID 731974노트

반응식

HRID 731974 반응식
C([O:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[C:15]([Cl:16])=[CH:14][C:13]([O:17][CH2:18][CH:19]=[C:20]([Cl:22])[Cl:21])=[CH:12][C:11]=1[Cl:23])(=O)C.[OH-].[Na+].O.Cl>CO>[Cl:22][C:20]([Cl:21])=[CH:19][CH2:18][O:17][C:13]1[CH:12]=[C:11]([Cl:23])[C:10]([O:9][CH2:8][CH2:7][CH2:6][CH2:5][OH:4])=[C:15]([Cl:16])[CH:14]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 184295004-[4-(3,3-Dichloroprop-2-enyloxy)-2,6-dichlorophenoxy]butyl acetate

생성물 1

HCID 222571304-{2,6-Dichloro-4-[(3,3-dichloroprop-2-EN-1-YL)oxy]phenoxy}butan-1-OL수율 93.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Twenty seven grams (0.067 mole) of 4-[4-(3,3-dichloroprop-2-enyloxy)-2,6-dichlorophenoxy]butyl acetate was stirred and a solution of 5.4 grams (0.134 mole) of sodium hydroxide in 300 mL of methanol was added portion-wise. Upon completion of addition the reaction mixture was stirred at ambient temperature during a two hour period. After this time the reaction mixture was stirred with 400 mL of water and was neutralized with concentrated hydrochloric acid. The neutral mixture was extracted with four 150 mL portions of diethyl ether, and the combined extracted were washed with one 150 mL portion of an aqueous solution saturated with sodium chloride. The organic layer was dried with sodium sulfate, filtered, and the filtrate was concentrated under reduced pressure to a residue, yielding 22.5 grams of the subject compound. The NMR spectrum was consistent with the proposed structure.

후처리

  1. additionUpon completion of addition the reaction mixture
  2. extractionThe neutral mixture was extracted with four 150 mL portions of diethyl ether
  3. extractionthe combined extracted
  4. washwere washed with one 150 mL portion of an aqueous solution saturated with sodium chloride
  5. dry with materialThe organic layer was dried with sodium sulfate
  6. filtrationfiltered
  7. concentrationthe filtrate was concentrated under reduced pressure to a residue

출처 및 근거

ORD 기록
ord-347d8882d6404375997f52f97fa89356
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07585891B2

반응 노트

불러오는 중…