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

HRID 497044ノート

反応式

HRID 497044 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 3283Diethyl Ether溶媒

反応条件

温度
85 °C

実験手順

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%)

後処理

  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

出典と根拠

ORDレコード
ord-0f40cc90efa04e9faed0a5a8808594e6
出典データセット
uspto-grants-2005_09
特許番号
US06949551B2

反応ノート

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