Hydrochloric Acid → 4-{[t-Butyl(diphenyl)silyl]oxy}-3-fluorophenol

HRID 1634734ノート

反応式

HRID 1634734 の反応式
C([O:4][C:5]1[CH:10]=[CH:9][C:8]([O:11][Si:12]([C:25]([CH3:28])([CH3:27])[CH3:26])([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[C:7]([F:29])[CH:6]=1)(=O)C.[OH-].[Na+].Cl>CO>[Si:12]([O:11][C:8]1[CH:9]=[CH:10][C:5]([OH:4])=[CH:6][C:7]=1[F:29])([C:25]([CH3:28])([CH3:27])[CH3:26])([C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 699857744-{[t-Butyl(diphenyl)silyl]oxy}-3-fluorophenyl acetate

生成物 1

HCID 699876834-{[t-Butyl(diphenyl)silyl]oxy}-3-fluorophenol収率 95%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

4-{[t -Butyl(diphenyl)silyl]oxy}-3-fluorophenyl acetate (5.28 g, 12.92 mmol) was dissolved in methanol (100 mL). 1N NaOH (15.5 mL) was added. The solution was stirred for 30 minutes at ambient temperature. 1N HCl (16 mL) was added. The solvent was removed in vacuo and the solid partitioned between dichloromethane and water. The aqueous phase was washed with dichloromethane. The organic layers were combined and the solvent dried over anhydrous magnesium sulfate. The solution was filtered and the solvent evaporated to dryness in vacuo to yield crude title compound (4.5 g, 12.28 mmol).

後処理

  1. customThe solvent was removed in vacuo
  2. customthe solid partitioned between dichloromethane and water
  3. washThe aqueous phase was washed with dichloromethane
  4. dry with materialthe solvent dried over anhydrous magnesium sulfate
  5. filtrationThe solution was filtered
  6. customthe solvent evaporated to dryness in vacuo

出典と根拠

ORDレコード
ord-4e14128c55344091b621e2ece53f2106
出典データセット
uspto-grants-2003_01
特許番号
US06506901B2

反応ノート

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