Water → 4-Methylthio-3-nitrobenzoic acid

HRID 1385034노트

반응식

HRID 1385034 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

HCID 5425314-Methylthio-3-nitrobenzoic acid

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
57.5 °C

실험 절차

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 to 55-60° 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.

후처리

  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

출처 및 근거

ORD 기록
ord-5d20f4cd72164840b85c93e272fe6fff
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06262074B1

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