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N-bromobutanimide → HCID 22721993, 화합물

HRID 1581508
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HRID 1581508 반응식
[NH2:1][C:2]1[C:3](=[O:14])[NH:4][N:5]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:7]=1.[Br:15]N1C(=O)CCC1=O>C(#N)C>[NH2:1][C:2]1[C:3](=[O:14])[NH:4][N:5]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:7]=1[Br:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 67184N-bromobutanimideHCID 105594874-amino-6-phenyl-2H-pyridazin-3-one

생성물 1

HCID 22721993HCID 22721993, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

4-Amino-6-phenyl-3(2H)-pyridazinone (prepared by the method of Example 1a), or according to McKillop et al., Heterocycles, 1989, 29(6), 1077) (4.69 g, 25 mmol) and N-bromosuccinimide (4.50 g, 25.3 mmol), suspended in dry acetonitrile (135 ml), was heated at reflux under a nitrogen atmosphere for 6 hours, then allowed to stand at room temperature for 18 hours. The solid was collected by filtration, washed with ethyl acetate (40 ml) and diethyl ether (40 ml), and dried in vacuo at 60° C., to afford the title compound, 6.25 g (94%), as a colourless solid. 1H NMR (400 MHz, DMSO-d6) δ12.93 (1H, s), 7.43 (5H, m), 6.69 (2H, br s); m/e (ES+) 266/268 [MH]+.

후처리

  1. temperaturewas heated
  2. temperatureat reflux under a nitrogen atmosphere for 6 hours
  3. filtrationThe solid was collected by filtration
  4. washwashed with ethyl acetate (40 ml) and diethyl ether (40 ml)
  5. customdried in vacuo at 60° C.

출처 및 근거

ORD 기록
ord-7df452dce7f44f9b902746957c0bb902
출처 데이터셋
uspto-grants-2004_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06730676B2

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