Dimethylamine methanol → N-[5-chloro-2-(dimethylsulfamoyl)benzyl]acetamide

HRID 1015749

反応式

HRID 1015749 の反応式
CO.[CH3:3][NH:4][CH3:5].[C:6]([NH:9][CH2:10][C:11]1[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:12]=1[S:18](Cl)(=[O:20])=[O:19])(=[O:8])[CH3:7]>CO.O1CCCC1>[Cl:17][C:15]1[CH:14]=[CH:13][C:12]([S:18](=[O:20])(=[O:19])[N:4]([CH3:5])[CH3:3])=[C:11]([CH:16]=1)[CH2:10][NH:9][C:6](=[O:8])[CH3:7]

参加物

5

反応物 2

HCID 22497844Dimethylamine methanolHCID 866508292-[(Acetylamino)methyl]-4-chlorobenzenesulfonyl chloride

生成物 1

HCID 66877112N-[5-chloro-2-(dimethylsulfamoyl)benzyl]acetamide

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

(Step 1) To a solution of 2N dimethylamine methanol solution (7.51 ml) in methanol (15 ml) was added dropwise a suspension of 2-[(acetylamino)methyl]-4-chlorobenzenesulfonyl chloride (2.12 g) in tetrahydrofuran (5 ml) under ice-cooling. The mixture was allowed to warm to room temperature, and stirred for 3 hr. The reaction mixture was quenched with water, and extracted with ethyl acetate. The extract was washed with saturated brine, and dried over magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate) to give N-[5-chloro-2-(dimethylsulfamoyl)benzyl]acetamide (1.77 g) as a white solid.

後処理

  1. temperaturecooling
  2. customThe reaction mixture was quenched with water
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (ethyl acetate)

出典と根拠

ORDレコード
ord-74ba9b8514fd47f9b611f683b5aeb474
出典データセット
uspto-grants-2011_07
特許番号
US07985862B2

関連ノート

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