Pyridine → N-(3-formylphenyl)methanesulfonamide

HRID 714465

반응식

HRID 714465 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([CH:8]=[O:9])[CH:5]=[CH:6][CH:7]=1.N1C=CC=CC=1.[CH3:16][S:17](Cl)(=[O:19])=[O:18].C(OCC)(=O)C>ClCCl>[CH:8]([C:4]1[CH:3]=[C:2]([NH:1][S:17]([CH3:16])(=[O:19])=[O:18])[CH:7]=[CH:6][CH:5]=1)=[O:9]

참가 물질

6

반응물 4

HCID 1049PyridineHCID 8857Ethyl AcetateHCID 31297Methanesulfonyl chlorideHCID 74366Benzaldehyde, 3-amino-

생성물 1

HCID 2794787N-(3-formylphenyl)methanesulfonamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1.3 g (10.73 mmol) of 3-aminobenzenecarbaldehyde were initially charged in 30 ml of dichloromethane. 849 mg (10.73 mmol) of pyridine and 1.3 g (10.73 mmol) of methanesulfonyl chloride were added, and the mixture was then stirred at RT overnight. Ethyl acetate was added, and the reaction solution was washed in each case once with 1 N hydrochloric acid, water and saturated aqueous sodium bicarbonate solution. The organic phase was dried over sodium sulfate, filtered and evaporated. The residue was purified by column chromatography on silica gel 60 (mobile phase: dichloromethane/methanol 100/0→50/1).

후처리

  1. washthe reaction solution was washed in each case once with 1 N hydrochloric acid, water and saturated aqueous sodium bicarbonate solution
  2. dry with materialThe organic phase was dried over sodium sulfate
  3. filtrationfiltered
  4. customevaporated
  5. customThe residue was purified by column chromatography on silica gel 60 (mobile phase: dichloromethane/methanol 100/0→50/1)

출처 및 근거

ORD 기록
ord-0ce1ef30f7a74835ba5753399bfa0386
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09187428B2

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