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

HRID 238968노트

반응식

HRID 238968 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][CH:23]=[C:22]([O:26][C:27]([F:30])([F:29])[F:28])[CH:21]=3)(=[O:19])=[O:18])[CH:11]=2)[CH2:6]1)=O.Cl>C(O)C>[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][CH:23]=[C:22]([O:26][C:27]([F:30])([F:28])[F:29])[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 689511843-[3-(3-Trifluoromethoxy-benzenesulfonylamino)-phenyl]-pyrrolidine-1-carboxylic acid methyl ester

생성물 1

HCID 68949003N-(3-Pyrrolidin-3-yl-phenyl)-3-trifluoromethoxy-benzenesulfonamide수율 48.5%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
120 °C

실험 절차

3-[3-(3-Trifluoromethoxy-benzenesulfonylamino)-phenyl]-pyrrolidine-1-carboxylic acid methyl ester (0.105 g; 0.24 mmol) were dissolved in 2.5 ml ethanol and 0.9 ml of concentrated HCl were added. The reaction mixture was heated in a microwave system (CEM) at 90-150° C. for several hours until consumption of starting material. The mixture was then concentrated in vacuo and the acidic aqueous phase extracted twice with diethylether. The aqueous phase was adjusted to pH 9 with 1 N aqueous NaOH, extracted three times with diethylether, and the combined organic layers dried over sodium sulfate, filtered and the solvent evaporated to dryness to yield 45 mg of the product.

후처리

  1. concentrationThe mixture was then concentrated in vacuo
  2. extractionthe acidic aqueous phase extracted twice with diethylether
  3. extractionextracted three times with diethylether
  4. dry with materialthe combined organic layers dried over sodium sulfate
  5. filtrationfiltered
  6. customthe solvent evaporated to dryness

출처 및 근거

ORD 기록
ord-bf39860572d5441ab6a39daa997349a0
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642642B2

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