Chloroacetone → 7-Chloro-3-methyl-1-benzothiophene

HRID 1380077ノート

反応式

HRID 1380077 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[SH:8].Cl[CH2:10][C:11](=O)[CH3:12]>[OH-].[Na+]>[Cl:1][C:2]1[C:3]2[S:8][CH:10]=[C:11]([CH3:12])[C:4]=2[CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 6571ChloroacetoneHCID 80599o-Chlorothiophenol

生成物 1

HCID 202421187-Chloro-3-methyl-1-benzothiophene

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

反応条件

温度
120 °C

実験手順

To a solution of 11.8 g. 2-chlorothiophenol (Aldrich, 15566-7) dissolved in aqueous sodium hydroxide (4.0 g./50 ml water) is added chloracetone (9.3 g.). After heating for 1 hour the reaction is cooled and extracted with methylene chloride. The extract is dried (MgSO4) and concentrated to an oil. The oil is added to polyphosphoric acid (100 g.) and slowly heated to 120° C. The mixture is added to ice and extracted with ethyl ether. The ether extract is washed with water (twice); dried (MgSO4) and concentrated to an oil. The oil is purified by distillation.

後処理

  1. temperatureAfter heating for 1 hour the reaction
  2. temperatureis cooled
  3. extractionextracted with methylene chloride
  4. dry with materialThe extract is dried (MgSO4)
  5. concentrationconcentrated to an oil
  6. additionThe oil is added to polyphosphoric acid (100 g.)
  7. additionThe mixture is added to ice
  8. extractionextracted with ethyl ether
  9. extractionThe ether extract
  10. washis washed with water (twice)
  11. dry with materialdried (MgSO4)
  12. concentrationconcentrated to an oil
  13. distillationThe oil is purified by distillation

出典と根拠

ORDレコード
ord-c34a80122c4e4924a7c39baded00cb9e
出典データセット
uspto-grants-1986_04
特許番号
US04579865

反応ノート

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