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

HRID 1241238노트

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HRID 1241238 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. The mixture was stirred for another 3 hours and 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 were dried and the solvent was removed. This gave 125.4 g (83%) of methyl 2-mercapto-4-chlorobenzoate.

후처리

  1. waitAfter 2 hours at this temperature
  2. temperaturethe mixture was cooled
  3. waitto stand at room temperature for 12 hours
  4. extractionextracted with ethyl acetate
  5. customthe combined organic phases were dried
  6. customthe solvent was removed

출처 및 근거

ORD 기록
ord-cfd27acc07684b6b8c7ec8e9f58ee4c1
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07115545B1

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