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Methylhydrazine → 4-(4-Bromophenyl)-2-methylphthalazin-1-one

HRID 54990
ノート
印刷プレビュー

反応式

HRID 54990 の反応式
[Br:1][C:2]1[CH:18]=[CH:17][C:5]([C:6]([C:8]2[CH:16]=[CH:15][CH:14]=[CH:13][C:9]=2[C:10](O)=[O:11])=O)=[CH:4][CH:3]=1.[CH3:19][NH:20][NH2:21]>C1(C)C=CC=CC=1>[CH3:19][N:20]1[N:21]=[C:6]([C:5]2[CH:17]=[CH:18][C:2]([Br:1])=[CH:3][CH:4]=2)[C:8]2[C:9](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:10]1=[O:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6061MethylhydrazineHCID 2560622-(4-Bromobenzoyl)benzoic acid

生成物 1

HCID 8388214-(4-Bromophenyl)-2-methylphthalazin-1-one収率 87%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a suspension of 2-(4-bromobenzoyl)benzoic acid (15.0 g, 49.2 mmol) in toluene (75 mL) at room temperature was added methylhydrazine (2.88 mL, 54.1 mmol). The reaction mixture was heated to reflux while collecting water in a Dean Stark trap for 3 hours, additional methylhydrazine (2.0 mL) was added and refluxing was continued for 15 minutes. The reaction mixture was cooled to room temperature and the product was collected by filtration and dried in vacuo to afford 13.4 g (87%) of 2-methyl-4-(4-bromophenyl)-1-(2H)-phthalazinone, m.p. 168°-170° C.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux
  3. customwhile collecting water in a Dean Stark trap for 3 hours
  4. additionadditional methylhydrazine (2.0 mL) was added
  5. temperaturerefluxing
  6. filtrationthe product was collected by filtration
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-c71224efa99e451d96777627c8179f4b
出典データセット
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05624922

反応ノート

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