2-Amino-2',5-dichlorobenzophenone → 2-[N-(4-Cyanophenylsulfonyl)amino]-2',5-dichlorobenzophenone
Reaktionsgleichung
[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]Komponenten
5
Versuchsvorschrift
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.
Aufarbeitung
- customthe mixture is evaporated to dryness, water and ethyl acetate
- additionare added
- washthe organic phase is washed
- additionwith dilute hydrochloric water, water
- dry with materialan aqueous solution of sodium chloride and dried over magnesium sulfate
- customthe solvent is evaporated off under vacuum
- customThe precipitate formed
- filtrationis filtered off
- customrecrystallized twice from a DCM/isopropyl ether mixture
Quellen und Nachweise
- ORD-Eintrag
- ord-978c6d95c6a84284942ba58e251a8191
- Quelldatensatz
- uspto-grants-1996_11
- Patentnummer
- US05578633
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