Methyl 4-chloro-2-(chlorosulphonyl)benzoate → 52948-12-6

HRID 1370168ノート

反応式

HRID 1370168 の反応式
Cl[S:2]([C:5]1[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:6]=1[C:7]([O:9][CH3:10])=[O:8])(=O)=O>Cl.[Zn]>[SH:2][C:5]1[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:6]=1[C:7]([O:9][CH3:10])=[O:8]

参加物

4

反応物 1

HCID 3020661Methyl 4-chloro-2-(chlorosulphonyl)benzoate

生成物 1

HCID 1565712452948-12-6

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 313Hydrochloric Acid溶媒

反応条件

温度
70 °C

実験手順

Over a period of 1.5 hours, 243.5 g (3.7 mol) of zinc powder were added a little at a time to a suspension of 205 g (0.75 mol) of methyl 2-chlorosulfonyl-4-chlorobenzoate in 1 l of concentrated hydrochloric acid and 375 g of ice. Stirring was continued for 3 hours, and the mixture was then slowly heated to 70° C. After 2 hours at this temperature, the mixture was cooled. The reaction mixture was allowed to stand at room temperature for 12 hours and then extracted with ethyl acetate, the combined organic phases [lacuna] and the solvent was removed. This gave 125.4 g (83%) of methyl 2-mercapto-4-chlorobenzoate.

後処理

  1. waitwas continued for 3 hours
  2. waitAfter 2 hours at this temperature
  3. temperaturethe mixture was cooled
  4. waitto stand at room temperature for 12 hours
  5. extractionextracted with ethyl acetate
  6. customthe combined organic phases [lacuna] and the solvent was removed

出典と根拠

ORDレコード
ord-71f1d83a0c8f4e129ab5dff463ef154e
出典データセット
uspto-grants-2003_06
特許番号
US06583089B1

反応ノート

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