Benzoyl chloride → N'-benzoyl-4-bromobenzohydrazide

HRID 1942976

反応式

HRID 1942976 の反応式
[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

参加物

4

反応物 2

HCID 7412Benzoyl chlorideHCID 222194-Bromobenzohydrazide2 回

生成物 1

HCID 3789270N'-benzoyl-4-bromobenzohydrazide収率 80%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒2 回

実験手順

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%).

後処理

  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%)

出典と根拠

ORDレコード
ord-950b9f6d8c4f4da59e41cb23d7b84875
出典データセット
uspto-grants-2013_03
特許番号
US08389735B2

関連ノート

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