Hydrochloric Acid → N-(3-Pyrrolidin-3-yl-phenyl)-4-trifluoromethoxy-benzenesulfonamide

HRID 1260226노트

반응식

HRID 1260226 반응식
COC([N:5]1[CH2:9][CH2:8][CH:7]([C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([NH:16][S:17]([C:20]3[CH:25]=[CH:24][C:23]([O:26][C:27]([F:30])([F:29])[F:28])=[CH:22][CH:21]=3)(=[O:19])=[O:18])[CH:11]=2)[CH2:6]1)=O.Cl>CCO>[NH:5]1[CH2:9][CH2:8][CH:7]([C:10]2[CH:11]=[C:12]([NH:16][S:17]([C:20]3[CH:25]=[CH:24][C:23]([O:26][C:27]([F:30])([F:28])[F:29])=[CH:22][CH:21]=3)(=[O:19])=[O:18])[CH:13]=[CH:14][CH:15]=2)[CH2:6]1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 574944463-[3-(4-Trifluoromethoxy-benzenesulfonylamino)-phenyl]-pyrrolidine-1-carboxylic acid methyl ester

생성물 1

HCID 60205208N-(3-Pyrrolidin-3-yl-phenyl)-4-trifluoromethoxy-benzenesulfonamide수율 46%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

3-[3-(4-Trifluoromethoxy-benzenesulfonylamino)-phenyl]-pyrrolidine-1-carboxylic acid methyl ester (500 mg, 1.13 mmol) and HCl (8M, 137.82 mmol) in EtOH (10 ml) were heated under reflux for 48 h. The mixture was extracted twice with ethyl acetate and then NaOH (2M) was added. The aqueous phase was extracted twice with ethyl acetate. The combined organic layers were washed with water and saturated sodium chloride solution, dried over MgSO4 and evaporated under reduced pressure to give the product as a brown oil (200 mg, 46%).

후처리

  1. temperatureunder reflux for 48 h
  2. extractionThe mixture was extracted twice with ethyl acetate
  3. additionNaOH (2M) was added
  4. extractionThe aqueous phase was extracted twice with ethyl acetate
  5. washThe combined organic layers were washed with water and saturated sodium chloride solution
  6. dry with materialdried over MgSO4
  7. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-b66e5f571bdf4dd7954e8758c6a5cf3b
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08470810B2

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