Dimethylformamide → 4-Chloro-4'-methylsulfonylmethylbenzophenone

HRID 2096

反応式

HRID 2096 の反応式
Br[CH2:2][C:3]1[CH:17]=[CH:16][C:6]([C:7]([C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=2)=[O:8])=[CH:5][CH:4]=1.[CH3:18][S:19]([O-:21])=[O:20].[Na+].CN(C)C=O>O>[Cl:15][C:12]1[CH:13]=[CH:14][C:9]([C:7]([C:6]2[CH:16]=[CH:17][C:3]([CH2:2][S:19]([CH3:18])(=[O:21])=[O:20])=[CH:4][CH:5]=2)=[O:8])=[CH:10][CH:11]=1

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 2733271Sodium methanesulfinateHCID 98396514-(4-Chlorobenzoyl)benzyl bromide

生成物 1

HCID 187799134-Chloro-4'-methylsulfonylmethylbenzophenone収率 90.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

4-bromomethyl-4'-chlorobenzophenone (3.1 g) and sodium methanesulfinate (1.5 g) were added to N,N-dimethylformamide (50 ml), and the mixture was stirred for 16 hours at room temperature. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with water and dried over anhydrous magnesium sulfate. Ethyl acetate was distilled off under reduced pressure. The residual solid was washed with n-hexane to obtain the desired product (2.8 g, melting point: 164° to 166° C., yield: 90%).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationEthyl acetate was distilled off under reduced pressure
  5. washThe residual solid was washed with n-hexane

出典と根拠

ORDレコード
ord-ade4f0eddda041248b4ac3c87079d5f2
出典データセット
uspto-grants-1998_03
特許番号
US05728699

関連ノート

読み込み中…