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

HRID 1383522

反応式

HRID 1383522 の反応式
[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]

参加物

3

反応物 2

HCID 74784-Methoxybenzoic AcidHCID 24638Chlorosulfonic acid

生成物 1

HCID 38548883-(Chlorosulfonyl)-4-methoxybenzoic acid

反応条件

温度
90 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4af61440a9034b86bc7a388f7506332a
出典データセット
uspto-grants-2001_07
特許番号
US06255326B1

関連ノート

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