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

HRID 1370168노트

반응식

HRID 1370168 반응식
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]

참가 물질

4

반응물 1

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

생성물 1

HCID 1565712452948-12-6

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 313Hydrochloric Acid용매

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-71f1d83a0c8f4e129ab5dff463ef154e
출처 데이터셋
uspto-grants-2003_06
특허 번호
US06583089B1

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