1,1,1-Trifluoro-2,4-pentanedione → 1-(2-Amino-4-(trifluoromethyl)thiazol-5-yl)ethanone

HRID 2801

反応式

HRID 2801 の反応式
OC1C(OS(C2C=CC(C)=CC=2)(=O)=O)=C(I)C=CC=1.[F:20][C:21]([F:29])([F:28])[C:22](=O)[CH2:23][C:24](=[O:26])[CH3:25].[NH2:30][C:31]([NH2:33])=[S:32]>C(#N)C>[C:24]([C:23]1[S:32][C:31]([NH2:33])=[N:30][C:22]=1[C:21]([F:29])([F:28])[F:20])(=[O:26])[CH3:25]

参加物

5

反応物 3

HCID 739431,1,1-Trifluoro-2,4-pentanedioneHCID 2723790ThioureaHCID 21918218Hydroxy tosyloxy iodobenzene

生成物 1

HCID 189363001-(2-Amino-4-(trifluoromethyl)thiazol-5-yl)ethanone

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Hydroxy(tosyloxy)iodobenzene (78.5 g) was added to a solution of 1,1,1-trifluoropentane-2,4-dione in acetonitrile (500 ml). The mixture was heated under reflux for 45 minutes, then cooled, and thiourea (15.2 g) was added. The mixture was heated under reflux for 4 hours and then left to stand overnight. Evaporation and crystallisation of the residue from dichloromethane gave the title compound.

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 45 minutes
  3. temperaturecooled
  4. temperatureThe mixture was heated
  5. temperatureunder reflux for 4 hours
  6. waitleft
  7. customEvaporation and crystallisation of the residue from dichloromethane

出典と根拠

ORDレコード
ord-ea8d9c1fc5de4b569364ab4d8c41abcc
出典データセット
uspto-grants-1998_03
特許番号
US05731335

関連ノート

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