Hydrochloric Acid → 2-Fluoro-5-hydroxy-4-methylphenol

HRID 393615ノート

反応式

HRID 393615 の反応式
C(=O)([O-])[O-].[K+].[K+].C(=O)(OC)[O:8][C:9]1[CH:14]=[C:13]([OH:15])[C:12]([F:16])=[CH:11][C:10]=1[CH3:17].Cl>CO>[F:16][C:12]1[CH:11]=[C:10]([CH3:17])[C:9]([OH:8])=[CH:14][C:13]=1[OH:15]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 22625031(4-Fluoro-5-hydroxy-2-methylphenyl) methyl carbonate

生成物 1

HCID 226465752-Fluoro-5-hydroxy-4-methylphenol収率 70.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

Potassium carbonate (870 mg, 6.3 mmol) was added to a solution of (4-fluoro-5-hydroxy-2-methylphenyl) methyl carbonate (1.2 g, 6 mmol) in methanol (20 ml) and the mixture was heated at 50° C. for 1 hour. The mixture was allowed to cool, adjusted to pH3 with hydrochloric acid and extracted with ethyl acetate. The combined extracts were washed with brine, dried (MgSO4) and the volatiles removed by evaporation. The residue was purified by column chromatography eluting with petroleum ether/ethyl acetate (7/3) to give 2-fluoro-5-hydroxy-4-methylphenol (603 mg, 70%) as a yellow solid.

後処理

  1. temperatureto cool
  2. extractionextracted with ethyl acetate
  3. washThe combined extracts were washed with brine
  4. dry with materialdried (MgSO4)
  5. customthe volatiles removed by evaporation
  6. customThe residue was purified by column chromatography
  7. washeluting with petroleum ether/ethyl acetate (7/3)

出典と根拠

ORDレコード
ord-35827393192649578d29c5c3ec8ece2a
出典データセット
uspto-grants-2004_10
特許番号
US06809097B1

反応ノート

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