Triethylamine → [5-Phenyl-4-(3-pyridyl)-1,3-thiazol-2-yl]amine

HRID 1167654ノート

反応式

HRID 1167654 の反応式
Br.Br[CH:3]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:4]([C:6]1[CH:7]=[N:8][CH:9]=[CH:10][CH:11]=1)=O.[NH2:18][C:19]([NH2:21])=[S:20].C(N(CC)CC)C>C(#N)C>[C:12]1([C:3]2[S:20][C:19]([NH2:21])=[N:18][C:4]=2[C:6]2[CH:7]=[N:8][CH:9]=[CH:10][CH:11]=2)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 2723790ThioureaHCID 134660052-Bromo-2-phenyl-1-(3-pyridyl)ethanone hydrobromide

生成物 1

HCID 9794996[5-Phenyl-4-(3-pyridyl)-1,3-thiazol-2-yl]amine収率 84%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
80 °C

実験手順

To a mixture of 2-bromo-2-phenyl-1-(3-pyridyl)ethanone hydrobromide (2.00 g) and thiourea (432 mg) in acetonitrile (30 mL), was added triethylamine (0.80 mL) dropwise and the resulting mixture was stirred at 80° C. for 3 h. The solvent was removed under reduced pressure and an aqueous saturated solution of sodium hydrogen carbonate was added to the residue. The mixture was extracted with ethyl acetate. The organic phases were washed with water, dried and concentrated under reduced pressure to give the amorphous title compound (1.10 g, yield 84%).

後処理

  1. customThe solvent was removed under reduced pressure
  2. additionan aqueous saturated solution of sodium hydrogen carbonate was added to the residue
  3. extractionThe mixture was extracted with ethyl acetate
  4. washThe organic phases were washed with water
  5. customdried
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-f82e8a8b3c1e4421941e83bc23fadfea
出典データセット
uspto-grants-2003_09
特許番号
US06620825B1

反応ノート

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