Water → 3-Acetyl-1-chloro-5-(3,3-dichloroprop-2-enyloxy)-2-hydroxybenzene

HRID 497044노트

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HRID 497044 반응식
[C:1]([C:4]1[C:5]([O:17]CC=C(Cl)Cl)=[C:6]([Cl:16])[CH:7]=[C:8]([O:10][CH2:11][CH:12]=[C:13]([Cl:15])[Cl:14])[CH:9]=1)(=[O:3])[CH3:2].O>C1(C)C=CC=CC=1.C(OCC)C>[C:1]([C:4]1[C:5]([OH:17])=[C:6]([Cl:16])[CH:7]=[C:8]([O:10][CH2:11][CH:12]=[C:13]([Cl:15])[Cl:14])[CH:9]=1)(=[O:3])[CH3:2]

참가 물질

5

반응물 2

HCID 962WaterHCID 223186103-Acetyl-2,5-bis-(3,3-dichloroprop-2-enyloxy)-1-chlorobenzene

생성물 1

HCID 114152013-Acetyl-1-chloro-5-(3,3-dichloroprop-2-enyloxy)-2-hydroxybenzene

시약·촉매·용매 2

HCID 1140Toluene용매HCID 3283Diethyl Ether용매

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온도
85 °C

실험 절차

6.1 g of 3-acetyl-2,5-bis-(3,3-dichloroprop-2-enyloxy)-1-chlorobenzene were dissolved in 160 ml of toluene. 7.79 g of magnesium dibromide/diethyl ether complex, dissolved in 25 ml of diethyl ether, were added to this solution, and the mixture was then stirred at 85° C. for 6 hours. After the reaction had ended according to TLC, the mixture was allowed to cool, about 300 ml of water were added and the organic phase was separated off. The aqueous phase was re-extracted twice with ethyl acetate, and the combined organic phases were then washed with saturated sodium chloride solution. After drying and concentration of the organic phase, the crude product was purified chromatographically. Yield: 2.86 g (64%)

후처리

  1. additionwere added to this solution
  2. temperatureto cool
  3. customthe organic phase was separated off
  4. extractionThe aqueous phase was re-extracted twice with ethyl acetate
  5. washthe combined organic phases were then washed with saturated sodium chloride solution
  6. customAfter drying
  7. customconcentration of the organic phase, the crude product was purified chromatographically

출처 및 근거

ORD 기록
ord-0f40cc90efa04e9faed0a5a8808594e6
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06949551B2

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