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

HRID 1769136
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HRID 1769136 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f6bafcda8e344961835216fe63e337b6
출처 데이터셋
uspto-grants-1995_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05380721

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