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

HRID 1468470ノート

反応式

HRID 1468470 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6902d52c34c04724a6c1cfadea210f36
出典データセット
uspto-grants-2015_04
特許番号
US09000108B2

反応ノート

読み込み中…