Triethylamine → HCID 11335869、化合物

HRID 1062628ノート

反応式

HRID 1062628 の反応式
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]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 2723790ThioureaHCID 11315915HCID 11315915、化合物

生成物 1

HCID 11335869HCID 11335869、化合物収率 70%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-711ccdfc223c4fdd90d91634aade00ed
出典データセット
uspto-grants-2005_11
特許番号
US06962933B1

反応ノート

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