1,3-Dibromopropane → 1,3-Bis(2,4-difluoro-6-iodophenoxy)propane

HRID 1468470노트

반응식

HRID 1468470 반응식
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[C:4]([I:9])[C:3]=1[OH:10].Br[CH2:12][CH2:13][CH2:14]Br.[C:16](=[O:19])([O-])[O-].[K+].[K+]>CC(C)=O>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[C:4]([I:9])[C:3]=1[O:10][CH2:12][CH2:13][CH2:14][O:19][C:16]1[C:4]([I:9])=[CH:3][C:2]([F:1])=[CH:7][C:6]=1[F:8]

참가 물질

5

반응물 3

HCID 80011,3-DibromopropaneHCID 11430Potassium CarbonateHCID 222216242,4-Difluoro-6-iodophenol

생성물 1

HCID 585165561,3-Bis(2,4-difluoro-6-iodophenoxy)propane

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a solution of 7.68 g (30 mmol) of 2,4-difluoro-6-iodophenol (P7), Preparation 7 and 3.03 g (15 mmol) of 1,3-dibromopropane in 125 mL of acetone add 12.42 g (90 mmol) of potassium carbonate. Reflux the resulting reaction mixture for 48 hours. Cool the reaction mixture to room temperature, filter it, and extract the resulting filtrate thoroughly with methylene chloride. Combine methylene chloride extracts and concentrate them by rotary evaporation. Crystallize the resulting solid from hexanes to yield 3.4 g (41.1%) of (P8) as a white solid.

후처리

  1. temperatureReflux
  2. customthe resulting reaction mixture for 48 hours
  3. filtrationfilter it
  4. extractionextract the resulting filtrate thoroughly with methylene chloride
  5. concentrationconcentrate them
  6. customby rotary evaporation
  7. customCrystallize the resulting solid from hexanes
  8. customto yield 3.4 g (41.1%) of (P8) as a white solid

출처 및 근거

ORD 기록
ord-6902d52c34c04724a6c1cfadea210f36
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09000108B2

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