2,6-Dibromo-4-trifluoromethoxyaniline → Thifluzamide

HRID 356644ノート

反応式

HRID 356644 の反応式
[CH3:1][C:2]1[S:3][C:4]([C:11](Cl)=[O:12])=[C:5]([C:7]([F:10])([F:9])[F:8])[N:6]=1.[Br:14][C:15]1[CH:21]=[C:20]([O:22][C:23]([F:26])([F:25])[F:24])[CH:19]=[C:18]([Br:27])[C:16]=1[NH2:17]>C(#N)C>[CH3:1][C:2]1[S:3][C:4]([C:11]([NH:17][C:16]2[C:18]([Br:27])=[CH:19][C:20]([O:22][C:23]([F:26])([F:24])[F:25])=[CH:21][C:15]=2[Br:14])=[O:12])=[C:5]([C:7]([F:10])([F:9])[F:8])[N:6]=1

参加物

4

反応物 2

HCID 27367972,6-Dibromo-4-trifluoromethoxyanilineHCID 146010812-Methyl-4-(trifluoromethyl)-5-thiazolecarbonyl chloride

生成物 1

HCID 86389Thifluzamide収率 98.9%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

2-Methyl-4-trifluoromethyl-5-chlorocarbonyl thiazole 6.47 g and 2,6-dibromo-4-trifluoromethoxy aniline 8.91 g were added in acetonitrile 16.8 ml, and they were heated to reflex for 6.5 hours. Solvent was removed from the reaction mixture by distillation under a reduced pressure, and then ethyl acetate 420 g and water 300 ml were added and they were agitated. After standing calmly, the ethyl acetate layer was collected, and washed with 300 ml each of water, saturated sodium bicarbonate solution, and water in succession. Then, after drying over anhydrous sodium sulfate, solvent was removed by distillation under a reduced pressure, to obtain thifluzamide 13.9 g.

後処理

  1. temperaturethey were heated
  2. customSolvent was removed from the reaction mixture by distillation under a reduced pressure
  3. additionethyl acetate 420 g and water 300 ml were added
  4. customthe ethyl acetate layer was collected
  5. washwashed with 300 ml each of water, saturated sodium bicarbonate solution, and water in succession
  6. dry with materialThen, after drying over anhydrous sodium sulfate, solvent
  7. customwas removed by distillation under a reduced pressure

出典と根拠

ORDレコード
ord-a638014f3cda413590fe5ed092f3690a
出典データセット
uspto-grants-1998_11
特許番号
US05837721

反応ノート

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