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

HRID 1380077노트

반응식

HRID 1380077 반응식
[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

참가 물질

4

반응물 2

HCID 6571ChloroacetoneHCID 80599o-Chlorothiophenol

생성물 1

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

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

반응 조건

온도
120 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c34a80122c4e4924a7c39baded00cb9e
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04579865

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