Water → 3-(3,5-Difluorophenyl)-1-propene

HRID 1995689ノート

反応式

HRID 1995689 の反応式
[CH2:1](Br)[CH:2]=[CH2:3].[F:5][C:6]1[CH:7]=[C:8](Br)[CH:9]=[C:10]([F:12])[CH:11]=1.[Mg].O>O1CCCC1>[CH2:3]([C:8]1[CH:7]=[C:6]([F:5])[CH:11]=[C:10]([F:12])[CH:9]=1)[CH:2]=[CH2:1]

参加物

6

反応物 4

HCID 962WaterHCID 7841Allyl bromideHCID 1363131-Bromo-3,5-difluorobenzeneHCID 5462224Magnesium

生成物 1

HCID 27583443-(3,5-Difluorophenyl)-1-propene

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

反応条件

温度
20 °C

実験手順

A solution of allyl bromide (2.5 g) in dry tetrahydorfuran (10 ml) was added dropwise with stirring to 3,5-difluorobromobenzene (4.0 g) with magnesium (0.5 g) in dry tetrahydrofuran) in dry tetrahydrofuran (40 ml), whilst maintaining the temperature of the mixture at about 20° C. When the addition was complete the mixture was allowed to warm to the ambient temperature (ca. 25° C.) After a period of 18 hours the mixture was poured into water (100 ml) and the resultant mixture extracted with diethyl ether, the extract washed with water, dried over anhydrous magnesium sulphate and the ether removed by distillation at atmospheric pressure. The residual oil was purified by distillation at atmospheric pressure to yield allyl-3,5-difluorobenzene (b.p. 154-155°) as a colourless oil.

後処理

  1. additionWhen the addition
  2. temperatureto warm to the ambient temperature (ca. 25° C.) After a period of 18 hours the mixture
  3. extractionthe resultant mixture extracted with diethyl ether
  4. washthe extract washed with water
  5. dry with materialdried over anhydrous magnesium sulphate
  6. customthe ether removed by distillation at atmospheric pressure
  7. distillationThe residual oil was purified by distillation at atmospheric pressure

出典と根拠

ORDレコード
ord-c171fe693bb8473fa17cf85cb264ebbb
出典データセット
uspto-grants-1983_09
特許番号
US04405640

反応ノート

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