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

HRID 343024

反応式

HRID 343024 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-d793c2a2e7fd45a1bccbeba3696812d1
出典データセット
uspto-grants-1999_01
特許番号
US05859283

関連ノート

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