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4'-Bromoacetanilide → Tert-butyl 2-({4-[(4-acetamidophenyl)ethynyl]phenyl}acetyl)hydrazinecarboxylate

HRID 1465432
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HRID 1465432 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(NC(C)C)(C)C.Br[C:28]1[CH:33]=[CH:32][C:31]([NH:34][C:35](=[O:37])[CH3:36])=[CH:30][CH:29]=1.[C:38]([C:40]1[CH:45]=[CH:44][C:43]([CH2:46][C:47]([NH:49][NH:50][C:51]([O:53][C:54]([CH3:57])([CH3:56])[CH3:55])=[O:52])=[O:48])=[CH:42][CH:41]=1)#[CH:39]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C(#N)C>[C:35]([NH:34][C:31]1[CH:32]=[CH:33][C:28]([C:39]#[C:38][C:40]2[CH:41]=[CH:42][C:43]([CH2:46][C:47]([NH:49][NH:50][C:51]([O:53][C:54]([CH3:57])([CH3:56])[CH3:55])=[O:52])=[O:48])=[CH:44][CH:45]=2)=[CH:29][CH:30]=1)(=[O:37])[CH3:36]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 76834'-BromoacetanilideHCID 7912DiisopropylamineHCID 11776TriphenylphosphineHCID 86651837Tert-butyl 2-[(4-ethynylphenyl)acetyl]hydrazinecarboxylate

생성물 1

HCID 67030024Tert-butyl 2-({4-[(4-acetamidophenyl)ethynyl]phenyl}acetyl)hydrazinecarboxylate수율 20.2%

시약·촉매·용매 2

HCID 167845
palladium(II) acetate
촉매
HCID 6342Acetonitrile용매

실험 절차

Palladium (II) acetate (2.5 mg, 0.011 mmol) and triphenylphosphine (11 mg, 0.044 mmol) were added to diisopropylamine (4 ml), and the mixture was stirred at room temperature for 20 mins. N-(4-Bromophenyl)acetamide (78 mg, 0.365 mmol) and tert-butyl 2-[(4-ethynylphenyl)acetyl]hydrazinecarboxylate (100 mg, 0.365 mmol) were added, and the mixture was stirred at 70° C. for 2 hrs. Anhydrous acetonitrile (2 ml) was added, and the mixture was further stirred at 70° C. for 1 hr. The reaction mixture was cooled and concentrated. The residue was purified by silica gel column chromatography (dichloromethane:methanol=97:3) to give tert-butyl 2-({4-[(4-acetamidophenyl)ethynyl]phenyl}acetyl)hydrazinecarboxylate (30 mg, yield 20%).

후처리

  1. stirringthe mixture was stirred at 70° C. for 2 hrs
  2. stirringthe mixture was further stirred at 70° C. for 1 hr
  3. temperatureThe reaction mixture was cooled
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel column chromatography (dichloromethane:methanol=97:3)

출처 및 근거

ORD 기록
ord-561813911a7543208f638708e7d94705
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08999989B2

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