Succinic anhydride → N-[2-[3-Chloro-4-(2-methylbenzoyl)-phenylamino]phenyl]-succinamic Acid

HRID 413515

Reaktionsgleichung

Reaktionsgleichung von HRID 413515
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][C:9]1[CH:23]=[CH:22][C:12]([C:13]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[CH3:21])=[O:14])=[C:11]([Cl:24])[CH:10]=1.[C:25]1(=[O:31])[O:30][C:28](=[O:29])[CH2:27][CH2:26]1>C(O)(=O)C>[Cl:24][C:11]1[CH:10]=[C:9]([NH:8][C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[NH:1][C:25](=[O:31])[CH2:26][CH2:27][C:28]([OH:30])=[O:29])[CH:23]=[CH:22][C:12]=1[C:13](=[O:14])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[CH3:21]

Komponenten

4

Edukt 2

HCID 7922Succinic anhydrideHCID 98191574-(2-Aminophenylamino)-2-chloro-2'-methylbenzophenone

Produkt 1

HCID 9845903N-[2-[3-Chloro-4-(2-methylbenzoyl)-phenylamino]phenyl]-succinamic Acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

A stirred solution of 4-(2-aminophenylamino)-2-chloro-2′-methylbenzophenone (3.0 mmol) in glacial acetic acid (5.0 ml) was heated to 70° C., then succinic anhydride (4.0 mmol) was added. The temperature was held at 100° C. for 20 min after which the reaction mixture was concentrated in vacuo to afford a light brown syrupy, which crystallised on standing. Trituration with a mixture of Et2O/CH2Cl2 3:1 followed by filtration and washing yielded the product as white crystals.

Aufarbeitung

  1. concentrationafter which the reaction mixture was concentrated in vacuo
  2. customto afford a light brown syrupy, which
  3. customcrystallised
  4. additionTrituration with a mixture of Et2O/CH2Cl2 3:1
  5. filtrationfollowed by filtration
  6. washwashing

Quellen und Nachweise

ORD-Eintrag
ord-270be73d92604e87855649e73eeb2f3f
Quelldatensatz
uspto-grants-2003_05
Patentnummer
US06566554B1

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