ar-Bromo-ar-nitrobenzenamine → HCID 131734569、化合物

HRID 595147

反応式

HRID 595147 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:6]=[C:7]([N+:9]([O-:11])=[O:10])[CH:8]=1)[NH2:5].Cl[C:13]1[N:18]=[C:17]([C:19]([F:22])([F:21])[F:20])[CH:16]=[CH:15][N:14]=1>O1CCOCC1>[Br:1][C:2]1[CH:3]=[C:4]([NH:5][C:13]2[N:18]=[C:17]([C:19]([F:22])([F:21])[F:20])[CH:16]=[CH:15][N:14]=2)[CH:6]=[C:7]([N+:9]([O-:11])=[O:10])[CH:8]=1

参加物

4

反応物 2

HCID 44535ar-Bromo-ar-nitrobenzenamineHCID 27739122-Chloro-4-(trifluoromethyl)pyrimidine

生成物 1

HCID 131734569HCID 131734569、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

was added to a solution of 3-bromo-5-nitroaniline (3.4 g, 15.7 mmol) and 2-chloro-4-(trifluoromethyl)pyrimidine) (2.27 mL, 18.80 mmol) in dioxane (78 ml) at room temperature, under nitrogen. The mixture became heterogeneous instantly and upon heating, a solution was obtained. The mixture was stirred at 100° C. for 18 hours then cooled to room temperature and concentrated under reduced pressure. Saturated sodium bicarbonate and dichloromethane were added, the organic phase was recovered using a phase separator and then concentrated under reduced pressure. The residue was washed in hexanes/ether and filtered to afford N-(3-bromo-5-nitrophenyl)-4-(trifluoromethyl)pyrimidin-2-amine.

後処理

  1. temperatureupon heating
  2. customa solution was obtained
  3. temperaturethen cooled to room temperature
  4. concentrationconcentrated under reduced pressure
  5. additionSaturated sodium bicarbonate and dichloromethane were added
  6. customthe organic phase was recovered
  7. concentrationconcentrated under reduced pressure
  8. washThe residue was washed in hexanes/ether
  9. filtrationfiltered

出典と根拠

ORDレコード
ord-6ad4c9f2656f41ba9b88245c8b6389b4
出典データセット
uspto-grants-2016_01
特許番号
US09242984B2

関連ノート

読み込み中…