Chlorosulfonic acid → 4-(Chlorosulfonyl)benzoic acid

HRID 263658ノート

反応式

HRID 263658 の反応式
[S:1]([C:5]1[CH:13]=[CH:12][C:8]([C:9]([OH:11])=[O:10])=[CH:7][CH:6]=1)(O)(=[O:3])=[O:2].[K].[Cl:15]S(O)(=O)=O>>[Cl:15][S:1]([C:5]1[CH:13]=[CH:12][C:8]([C:9]([OH:11])=[O:10])=[CH:7][CH:6]=1)(=[O:3])=[O:2]

参加物

3

反応物 2

HCID 24638Chlorosulfonic acidHCID 162119824-Sulfobenzoic acid monopotassium salt

生成物 1

HCID 823854-(Chlorosulfonyl)benzoic acid

反応条件

温度
100 °C

実験手順

4-Chlorosulfonylbenzoic acid is prepared by procedures described in (J. Chem. Soc., Vol. 121, 2022-26, 1922). A 250 mL flask equipped with condenser, CaCl2 drying tube and magnetic stirrer is charged with 35.1 g (0.146 mol) of potassium 4-sulfobenzoic acid and 50 mL of chlorosulfonic acid. The flask is placed in an oil bath and warmed to 100° C. After 1 hour at temperature, the reaction mixture is homogeneous. The reaction mixture is cooled and poured onto 300 g of crushed ice. The white precipitate is collected by filtration and washed 3 times with 100 mL portions of cold water. After air drying the solid is placed in a vacuum oven at 65° C. to yield 26.7 g of 4-chlorosulfonyl benzoic acid.

後処理

  1. custom4-Chlorosulfonylbenzoic acid is prepared by procedures
  2. customA 250 mL flask equipped with condenser, CaCl2 drying tube and magnetic stirrer
  3. customThe flask is placed in an oil bath
  4. temperatureThe reaction mixture is cooled
  5. filtrationThe white precipitate is collected by filtration
  6. washwashed 3 times with 100 mL portions of cold water
  7. customAfter air drying the solid
  8. customis placed in a vacuum oven at 65° C.

出典と根拠

ORDレコード
ord-ec4d4fff87ca45b3a9342fca35014bfe
出典データセット
uspto-grants-1997_07
特許番号
US05644017

反応ノート

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