Pyridine → N-(3-formylphenyl)methanesulfonamide

HRID 714465

反応式

HRID 714465 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 2794787N-(3-formylphenyl)methanesulfonamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-0ce1ef30f7a74835ba5753399bfa0386
出典データセット
uspto-grants-2015_11
特許番号
US09187428B2

関連ノート

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