4-Methoxybenzoic Acid → 3-(Chlorosulfonyl)-4-methoxybenzoic acid

HRID 356939노트

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HRID 356939 반응식
[C:1]([OH:11])(=[O:10])[C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][CH:3]=1.[Cl:12][S:13](O)(=[O:15])=[O:14]>>[Cl:12][S:13]([C:6]1[CH:7]=[C:2]([CH:3]=[CH:4][C:5]=1[O:8][CH3:9])[C:1]([OH:11])=[O:10])(=[O:15])=[O:14]

참가 물질

3

반응물 2

HCID 74784-Methoxybenzoic AcidHCID 24638Chlorosulfonic acid

생성물 1

HCID 38548883-(Chlorosulfonyl)-4-methoxybenzoic acid

반응 조건

온도
90 °C

실험 절차

A stirred solution of chlorosulfonic acid (90 mL) at room temperature is treated with p-anisic acid (40 g), portionwise, during 30 minutes. When the addition is complete, the mixture is stirred at 90° C. for 75 minutes, then it is cooled and poured onto ice. The white precipitate is collected and dissolved in ethyl acetate (300 mL). The organic extract is washed with brine (2×250 mL), dried over magnesium sulfate, and concentrated, to give 3-chlorosulfonyl-4-methoxybenzoic acid (34 g), in the form of a white solid m.p. 168°-170° C.

후처리

  1. additionWhen the addition
  2. temperatureit is cooled
  3. additionpoured onto ice
  4. customThe white precipitate is collected
  5. dissolutiondissolved in ethyl acetate (300 mL)
  6. extractionThe organic extract
  7. washis washed with brine (2×250 mL)
  8. dry with materialdried over magnesium sulfate
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b4dc8474cf184bdaa9771d2c876fed48
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840724

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