2-Amino-2',5-dichlorobenzophenone → 2-[N-(4-Cyanophenylsulfonyl)amino]-2',5-dichlorobenzophenone

HRID 374631노트

반응식

HRID 374631 반응식
[NH2:1][C:2]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[Cl:12])=[O:5].[C:18]([C:20]1[CH:25]=[CH:24][C:23]([S:26](Cl)(=[O:28])=[O:27])=[CH:22][CH:21]=1)#[N:19]>N1C=CC=CC=1.CN(C1C=CN=CC=1)C>[C:18]([C:20]1[CH:21]=[CH:22][C:23]([S:26]([NH:1][C:2]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:3]=2[C:4]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[Cl:12])=[O:5])(=[O:28])=[O:27])=[CH:24][CH:25]=1)#[N:19]

참가 물질

5

반응물 2

HCID 180692-Amino-2',5-dichlorobenzophenoneHCID 394974-Cyanobenzenesulfonyl chloride

생성물 1

HCID 233687202-[N-(4-Cyanophenylsulfonyl)amino]-2',5-dichlorobenzophenone

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 1049Pyridine용매

실험 절차

10 g of 2-amino-2',5-dichlorobenzophenone and 7.7 g of 4-cyanophenylsulfonyl chloride are heated in pyridine at 100° C. for 48 hours in the presence of 4.6 g of DMAP, the mixture is evaporated to dryness, water and ethyl acetate are added, the organic phase is washed with dilute hydrochloric water, water and an aqueous solution of sodium chloride and dried over magnesium sulfate and the solvent is evaporated off under vacuum. The precipitate formed is filtered off and then recrystallized twice from a DCM/isopropyl ether mixture to give the expected product.

후처리

  1. customthe mixture is evaporated to dryness, water and ethyl acetate
  2. additionare added
  3. washthe organic phase is washed
  4. additionwith dilute hydrochloric water, water
  5. dry with materialan aqueous solution of sodium chloride and dried over magnesium sulfate
  6. customthe solvent is evaporated off under vacuum
  7. customThe precipitate formed
  8. filtrationis filtered off
  9. customrecrystallized twice from a DCM/isopropyl ether mixture

출처 및 근거

ORD 기록
ord-47f7c9609c0b47858997b9c08e6665a8
출처 데이터셋
uspto-grants-1996_01
특허 번호
US05481005

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