Sulfuric Acid → 2-(2-Chloro-6-fluorophenyl)-propene

HRID 1288768노트

반응식

HRID 1288768 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[C:9](O)([CH3:11])[CH3:10].S(=O)(=O)(O)O>O>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[C:9]([CH3:11])=[CH2:10]

참가 물질

4

반응물 2

HCID 1118Sulfuric AcidHCID 540290942-(2-Chloro-6-fluorophenyl)propan-2-ol

생성물 1

HCID 543491142-(2-Chloro-6-fluorophenyl)-propene수율 67.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 2-(2-chloro-6-fluorophenyl)propan-2-ol (19.0 g), concentrated sulphuric acid and water was heated at reflux for 2 hours. It was cooled and extracted with ether, washed with water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness and the residue was purified by chromatography eluted with hexane to give 2-(2-chloro-6-fluorophenyl)-propene (11.6 g) as a clear oil, NMR (CDCl3) 1.95(s,3H) 4.95(s,1H), 5.85(s,1H), 6.85-7.0(m,1H), 7.05-7.2(m,2H).

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 2 hours
  3. temperatureIt was cooled
  4. extractionextracted with ether
  5. washwashed with water
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. customThe filtrate was evaporated to dryness
  9. customthe residue was purified by chromatography
  10. washeluted with hexane

출처 및 근거

ORD 기록
ord-76553f1e0c9a4cfd8f9746132ff4ba19
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05747424

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