Triethylamine → HCID 11335869, 화합물

HRID 1062628노트

반응식

HRID 1062628 반응식
Br.Br[CH:3]([C:16]1[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=1)[C:4]([C:6]1[CH:11]=[CH:10][C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])=[CH:8][CH:7]=1)=O.[NH2:22][C:23]([NH2:25])=[S:24].C(N(CC)CC)C>C(#N)C>[CH3:13][C:12]([C:9]1[CH:10]=[CH:11][C:6]([C:4]2[N:22]=[C:23]([NH2:25])[S:24][C:3]=2[C:16]2[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=2)=[CH:7][CH:8]=1)([CH3:15])[CH3:14]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 2723790ThioureaHCID 11315915HCID 11315915, 화합물

생성물 1

HCID 11335869HCID 11335869, 화합물수율 70%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of 2-bromo-1-[4-(1,1-dimethylethyl)phenyl]-2-(4-pyridyl)ethanone hydrobromide (5.0 g, 12 mmol) and thiourea (0.95 g, 13 mmol) in acetonitrile (60 mL) was added dropwise triethylamine (1.8 ml, 13 mmol) and the mixture was refluxed for 3 h. The solvent was evaporated under reduced pressure and saturated aqueous sodium hydrogencarbonate solution was added to the residue. The precipitated solid was collected by filtration. The obtained crude crystal was recrystallized from ethanol to give the title compound (2.6 g, 8.4 mmol, yield 69%).

후처리

  1. temperaturethe mixture was refluxed for 3 h
  2. customThe solvent was evaporated under reduced pressure and saturated aqueous sodium hydrogencarbonate solution
  3. additionwas added to the residue
  4. filtrationThe precipitated solid was collected by filtration
  5. customThe obtained crude crystal
  6. customwas recrystallized from ethanol

출처 및 근거

ORD 기록
ord-711ccdfc223c4fdd90d91634aade00ed
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06962933B1

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