ar-Bromo-ar-nitrobenzenamine → HCID 131734569, 화합물

HRID 595147

반응식

HRID 595147 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 131734569HCID 131734569, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6ad4c9f2656f41ba9b88245c8b6389b4
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09242984B2

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