Iodine → 4-Bromo-2-iodo-5-(trifluoromethyl)aniline

HRID 513850

반응식

HRID 513850 반응식
[I:1]I.[Br:3][C:4]1[CH:10]=[CH:9][C:7]([NH2:8])=[CH:6][C:5]=1[C:11]([F:14])([F:13])[F:12]>S([O-])([O-])(=O)=O.[Ag+2].C(O)C>[Br:3][C:4]1[C:5]([C:11]([F:12])([F:13])[F:14])=[CH:6][C:7]([NH2:8])=[C:9]([I:1])[CH:10]=1

참가 물질

5

반응물 2

HCID 807IodineHCID 678524-Bromo-3-(trifluoromethyl)aniline

생성물 1

HCID 455880634-Bromo-2-iodo-5-(trifluoromethyl)aniline

시약·촉매·용매 2

HCID 178418844HCID 178418844, 화합물촉매HCID 702Ethanol용매

실험 절차

Iodine (1.4 g, 5.5 mmol, 1.1 eq.) was gradually added to a mixture solution of 4-bromo-3-trifluoromethyl aniline (1.2 g, 1.0 mmol), silver sulfate (1.72 g, 5.5 mmol, 1.1 eq.), and anhydrous ethanol (35 ml). This was stirred at room temperature for two and half hours. The reaction mixture was filtered through Celite, and washed with ethyl acetate. The wash solution was washed with aqueous solutions of 10% sodium thiosulfate, saturated sodium bicarbonate, and saturated sodium chloride, and then dried over anhydrous sodium sulfate. The desiccant was removed by filtration, and concentration was performed. Crude solid 4-bromo-2-iodo-5-trifluoromethyl-phenylamine was obtained by concentration under reduced pressure. The resulting crude product was used in subsequent reactions without being purified.

후처리

  1. filtrationThe reaction mixture was filtered through Celite
  2. washwashed with ethyl acetate
  3. washThe wash solution was washed with aqueous solutions of 10% sodium thiosulfate, saturated sodium bicarbonate, and saturated sodium chloride
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe desiccant was removed by filtration, and concentration

출처 및 근거

ORD 기록
ord-a22897a594704894a4d0c627c0fb8bfc
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09102692B2

연결된 노트

불러오는 중…