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Hydrochloric Acid → HCID 178447829、化合物

HRID 857602
ノート
印刷プレビュー

反応式

HRID 857602 の反応式
[Li].[F:2][C:3]1[C:12]([F:13])=[CH:11][CH:10]=[C:9]2[C:4]=1[CH:5]=[CH:6][C:7](Br)=[CH:8]2.I[C:16]1[CH:21]=[CH:20][C:19]([C@H:22]2[CH2:27][CH2:26][C@H:25]([CH2:28][CH2:29][CH3:30])[CH2:24][CH2:23]2)=[CH:18][CH:17]=1.Cl>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1COCC1>[F:2][C:3]1[C:12]([F:13])=[CH:11][CH:10]=[C:9]2[C:4]=1[CH:5]=[CH:6][C:7]([C:16]1[CH:17]=[CH:18][C:19]([C@H:22]3[CH2:27][CH2:26][C@H:25]([CH2:28][CH2:29][CH3:30])[CH2:24][CH2:23]3)=[CH:20][CH:21]=1)=[CH:8]2
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 3028194LithiumHCID 114138325,6-Difluoro-2-bromonaphthaleneHCID 178447892HCID 178447892、化合物

生成物 1

HCID 178447829HCID 178447829、化合物

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物
触媒
HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a THF solution of an organic lithium reagent prepared from 5,6-difluoro-2-bromonaphthalene were added dropwise 4-iodo-1-(trans-4-propylcyclohexyl)benzene and a THF solution of tetrakis(triphenylphosphine)palladium (0) in the catalytic amount. The reaction mixture was then stirred at room temperature for 3 hours. To the reaction mixture were then added water and toluene to terminate the reaction. To the reaction solution was then added diluted hydrochloric acid until the aqueous phase became weakly acidic. The reaction solution was then extracted with toluene. The material thus extracted and the organic phase were together washed with water and then with saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain an oily matter. The oily matter was purified through silica gel column chromatography (hexane), and then recrystallized from ethanol to obtain 5,6-difluoro-2-[4-(trans-4-propylcyclohexyl)phenyl]naphthalene in the form of white crystal.

後処理

  1. customadded water and toluene to terminate
  2. customthe reaction
  3. extractionThe reaction solution was then extracted with toluene
  4. extractionThe material thus extracted
  5. washthe organic phase were together washed with water
  6. dry with materialwith saturated brine, and then dried over anhydrous sodium sulfate
  7. distillationThe solvent was distilled off under reduced pressure
  8. customto obtain an oily matter
  9. customThe oily matter was purified through silica gel column chromatography (hexane)
  10. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-d5b64def43d848078631c8d3994f0c1f
出典データセット
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07145047B2

反応ノート

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