Water → 4-Methylthio-3-nitrobenzoic acid

HRID 1017124ノート

反応式

HRID 1017124 の反応式
F[C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[N+:11]([O-:13])=[O:12].C[O-].[Na+].[CH3:17][S-:18].[Na+].O>CO>[N+:11]([C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][C:2]=1[S:18][CH3:17])[C:6]([OH:8])=[O:7])([O-:13])=[O:12]

参加物

6

反応物 4

HCID 962WaterHCID 679874-Fluoro-3-nitrobenzoic acidHCID 4378561Sodium methanethiolateHCID 10942334Sodium Methoxide

生成物 1

HCID 5425314-Methylthio-3-nitrobenzoic acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
57.5 °C

実験手順

0.75 mol of 4-fluoro-3-nitrobenzoic acid was charged in 2 l of methanol, and 0.75 mol of sodium methoxide was added dropwise. 0.83 mol of sodium thiomethoxide was then added and the reaction mixture was heated at from 55 to 60° C. for 5 hours. After cooling, 1 l of water was added, the precipitate was filtered off with suction and washed with 100 ml of methylene chloride. The residue was then taken up in 500 ml of 2 N hydrochloric acid and the precipitate formed was filtered off with suction and washed with water. The residue was then taken up in tetrahydrofuran and dried over sodium sulfate and the solvent was distilled off.

後処理

  1. temperatureAfter cooling
  2. filtrationthe precipitate was filtered off with suction
  3. washwashed with 100 ml of methylene chloride
  4. customthe precipitate formed
  5. filtrationwas filtered off with suction
  6. washwashed with water
  7. dry with materialdried over sodium sulfate
  8. distillationthe solvent was distilled off

出典と根拠

ORDレコード
ord-f985cc9ac96c4c3585c6216d8ba41370
出典データセット
uspto-grants-2002_11
特許番号
US06479436B1

反応ノート

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