Water → 3-(Methylthio)-4-nitrophenol

HRID 1402986ノート

反応式

HRID 1402986 の反応式
F[C:2]1[CH:3]=[C:4]([OH:11])[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9].[CH3:12][S-:13].[Na+].C(=O)([O-])[O-].[K+].[K+].O>CN(C=O)C>[CH3:12][S:13][C:2]1[CH:3]=[C:4]([OH:11])[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 5209483-Fluoro-4-nitrophenolHCID 4378561Sodium methanethiolate

生成物 1

HCID 441857023-(Methylthio)-4-nitrophenol収率 90.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 3-fluoro-4-nitrophenol (2 g, 12.7 mmol) in dry DMF (67 mL) were added by aliquots 2 equivalents of sodium thiomethoxide (1.78 g, 25.5 mmol) followed by 3 equivalents of potassium carbonate (5.27 g, 38.2 mmol). The mixture was stirred at RT for 23 hours and then water (100 mL) was added. The mixture was extracted with EtOAc, and the combined organic layers washed successively with water (60 mL) and brine (60 mL) and then dried over MgSO4. The solvent was evaporated under vacuum to provide the title compound (2.12 g, 90%) as a yellow powder.

後処理

  1. extractionThe mixture was extracted with EtOAc
  2. washthe combined organic layers washed successively with water (60 mL) and brine (60 mL)
  3. dry with materialdried over MgSO4
  4. customThe solvent was evaporated under vacuum

出典と根拠

ORDレコード
ord-31bb693455614cdeb1e79e8be71161fc
出典データセット
uspto-grants-2014_12
特許番号
US08912191B2

反応ノート

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