Dimethylformamide → 4-Chloro-4'-methylsulfonylmethylbenzophenone

HRID 2096

반응식

HRID 2096 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 187799134-Chloro-4'-methylsulfonylmethylbenzophenone수율 90.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-ade4f0eddda041248b4ac3c87079d5f2
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728699

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