Hydrochloric Acid → 3-Chloro-o-cresol

HRID 21833

反応式

HRID 21833 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[CH3:11].Cl>CN(C=O)C>[Cl:9][C:4]1[C:3]([CH3:11])=[C:2]([OH:8])[CH:7]=[CH:6][CH:5]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 189709711,3,3-Trichloro-2-methyl-7-oxabicyclo[4.1.0]heptane

生成物 1

HCID 148563-Chloro-o-cresol収率 89.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2 g (9.28 mmol) of epoxide 2h in solution in 5 cm3 of anhydrous DMF were heated to reflux for 3 h. The solution was acidified (pH=1) with 3N HCl, extracted with ether (4×25 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). 1.18 g of phenol 4e were obtained (macrobore GC purity>96%). The yield of compound 4e was 89%.

後処理

  1. temperatureto reflux for 3 h
  2. extractionextracted with ether (4×25 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-1ac2c1865d0a4e33a67f9b64d9f725a8
出典データセット
uspto-grants-1995_06
特許番号
US05424460

関連ノート

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