1,3-Dibromopropane → 1,3-Bis(4-fluoro-2-iodophenoxy)propane

HRID 572953노트

반응식

HRID 572953 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([I:9])[CH:3]=1.Br[CH2:11][CH2:12][CH2:13]Br.[C:15](=[O:18])([O-])[O-].[K+].[K+]>CC(C)=O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:11][CH2:12][CH2:13][O:18][C:15]2[CH:6]=[CH:7][C:2]([F:1])=[CH:3][C:4]=2[I:9])=[C:4]([I:9])[CH:3]=1

참가 물질

5

반응물 3

HCID 80011,3-DibromopropaneHCID 11430Potassium CarbonateHCID 101714174-Fluoro-2-iodophenol

생성물 1

HCID 667805951,3-Bis(4-fluoro-2-iodophenoxy)propane

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a solution of 15.00 g (63.03 mmol) of 4-fluoro-2-iodophenol (P7), Preparation 7 and 6.40 g (31.68 mmol) of 1,3-dibromopropane in 200 mL of acetone add 26.00 g (188.4 mmol) of potassium carbonate. Reflux the resulting reaction mixture for 24 hours. Cool the reaction mixture to room temperature, filter it, and concentrate the filtrate by rotary evaporation. Crystallize the resulting solid from acetonitrile to yield 12.00 g (74%) of (P8) as a white crystalline solid.

후처리

  1. temperatureReflux
  2. customthe resulting reaction mixture for 24 hours
  3. filtrationfilter it
  4. concentrationconcentrate the filtrate
  5. customby rotary evaporation
  6. customCrystallize the resulting solid from acetonitrile
  7. customto yield 12.00 g (74%) of (P8) as a white crystalline solid

출처 및 근거

ORD 기록
ord-d97b5df56a5a4d84ba81625083555a2a
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09029487B2

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