Benzoyl chloride → N'-benzoyl-4-bromobenzohydrazide

HRID 1942976

Reaktionsgleichung

Reaktionsgleichung von HRID 1942976
[Br:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([NH:8][NH2:9])=[O:7])=[CH:4][CH:3]=1.[C:12](Cl)(=[O:19])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>CN1CCCC1=O>[C:12]([NH:9][NH:8][C:6](=[O:7])[C:5]1[CH:10]=[CH:11][C:2]([Br:1])=[CH:3][CH:4]=1)(=[O:19])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

Komponenten

4

Edukt 2

HCID 7412Benzoyl chlorideHCID 222194-Bromobenzohydrazide2×

Produkt 1

HCID 3789270N'-benzoyl-4-bromobenzohydrazideAusbeute 80 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 13387N-methyl-2-pyrrolidoneLösungsmittel2×

Versuchsvorschrift

Subsequently, 2.0 g (13.9 mmol) of the 4-bromobenzohydrazide obtained in (i) above was put in a 300-mL three-neck flask, 7 mL of N-methyl-2-pyrrolidone (abbreviation: NMP) was added therein, and the mixture was stirred. Thereafter, a mixture of 2.5 mL of N-methyl-2-pyrrolidone and 2.5 mL (21.5 mmol) of benzoyl chloride was dripped through a 50-mL dropping funnel, and the mixture was stirred at 80° C. for 3 hours. The obtained solid was washed with water and a sodium carbonate aqueous solution in this order and collected by suction filtration. Then, the solid was recrystallized with acetone; thus, 3.6 g of a white solid of 1-benzoyl-2-(4-bromobenzoyl)hydrazine that was an object was obtained (yield: 80%).

Aufarbeitung

  1. customabove was put in a 300-mL three-neck flask
  2. stirringthe mixture was stirred at 80° C. for 3 hours
  3. washThe obtained solid was washed with water
  4. filtrationa sodium carbonate aqueous solution in this order and collected by suction filtration
  5. customThen, the solid was recrystallized with acetone
  6. customwas obtained (yield: 80%)

Quellen und Nachweise

ORD-Eintrag
ord-950b9f6d8c4f4da59e41cb23d7b84875
Quelldatensatz
uspto-grants-2013_03
Patentnummer
US08389735B2

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