Hydrochloric Acid → 3-Chloro-2-vinylphenol

HRID 21834ノート

反応式

HRID 21834 の反応式
Cl[C:2]12[O:8][CH:7]1[CH2:6][CH2:5][C:4](Cl)([Cl:9])[CH:3]2[CH:11]=[CH2:12].Cl>CN(C=O)C>[Cl:9][C:4]1[C:3]([CH:11]=[CH2:12])=[C:2]([OH:8])[CH:7]=[CH:6][CH:5]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 189709491,3,3-Trichloro-2-vinyl-7-oxabicyclo[4.1.0]heptane

生成物 1

HCID 189709553-Chloro-2-vinylphenol収率 75.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

0.84 g (3.69 mmol) of epoxide 2i in solution in 4 cm3 of anhydrous DMF were heated to reflux for 3 h 30 min. The solution was acidified (pH=1) with 3N HCl, extracted with ether (4×20 cm3), dried over MgSO4, filtered and evaporated down. The crude product obtained was purified by flash chromatography on silica (eluent: ether/petroleum ether=5/95). 0.43 g of phenol 4f were obtained (macrobore GC purity>99%). The yield of compound 4f was 75.5%.

後処理

  1. temperatureto reflux for 3 h 30 min
  2. extractionextracted with ether (4×20 cm3)
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. customevaporated down
  6. customThe crude product obtained
  7. customwas purified by flash chromatography on silica (eluent: ether/petroleum ether=5/95)

出典と根拠

ORDレコード
ord-8925bd503a8e4c209a12c8bb9fb832aa
出典データセット
uspto-grants-1995_06
特許番号
US05424460

反応ノート

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