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

HRID 1901803ノート

反応式

HRID 1901803 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-978c6d95c6a84284942ba58e251a8191
出典データセット
uspto-grants-1996_11
特許番号
US05578633

反応ノート

読み込み中…