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

HRID 1260226ノート

反応式

HRID 1260226 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-b66e5f571bdf4dd7954e8758c6a5cf3b
出典データセット
uspto-grants-2013_06
特許番号
US08470810B2

反応ノート

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