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

HRID 266580

反応式

HRID 266580 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 543491142-(2-Chloro-6-fluorophenyl)-propene収率 67.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-a507d08a3b8841fd851649d7b150fc81
出典データセット
uspto-grants-1997_07
特許番号
US05650533

関連ノート

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