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Cyclohexyl methyl ketone → 1-Cyclohexyl-2-(4-cyclohexyloxy-phenyl)-ethanone

HRID 2168708
ノート
印刷プレビュー

反応式

HRID 2168708 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([O:8][CH:9]2[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]2)=[CH:4][CH:3]=1.[CH:15]1([C:21]([CH3:23])=[O:22])[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1.C1C=CC(P(C2C=CC3C(=CC=CC=3)C=2C2C3C(=CC=CC=3)C=CC=2P(C2C=CC=CC=2)C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.CC(C)([O-])C.[K+]>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[CH:15]1([C:21](=[O:22])[CH2:23][C:2]2[CH:7]=[CH:6][C:5]([O:8][CH:9]3[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]3)=[CH:4][CH:3]=2)[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 13207Cyclohexyl methyl ketoneHCID 634876Binap, (A+-)-HCID 111397141-Bromo-4-(cyclohexyloxy)benzeneHCID 23665647Potassium tert-butoxide

生成物 1

HCID 673746771-Cyclohexyl-2-(4-cyclohexyloxy-phenyl)-ethanone収率 29.7%

試薬・触媒・溶媒 1

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒

反応条件

温度
90 °C

実験手順

A stirred suspension of 1-bromo-4-cyclohexyloxy-benzene (3.92 mmol, 1.0 g), cyclohexylmethylketone (5.92 mmol, 0.83 mL), (R)-(+)-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (1.88 mmol, 1.17 g), tris(dibenzylideneacetone)dipalladium(0) (0.78 mmol, 0.72 g), and potassium t-butoxide (7.84 mmol, 0.88 g) were heated to 90° C. for 12 h in a sealed vial. The reaction was cooled and partitioned in water (50 mL) and diethyl ether (50 mL). The mixture was filtered through fluted filter paper and the layers were separated. The aqueous layer was washed with diethyl ether (3×20 mL). The combined organic layers were washed with brine (10 mL), dried (Na2SO4), filtered, and concentrated under reduced pressure. The crude product was purified on a 24 g SiO2 cartridge using an ethyl acetate/hexanes gradient to give 1-cyclohexyl-2-(4-cyclohexyloxy-phenyl)-ethanone (0.35 g).

後処理

  1. temperatureThe reaction was cooled
  2. custompartitioned in water (50 mL)
  3. filtrationThe mixture was filtered
  4. filtrationthrough fluted filter paper
  5. customthe layers were separated
  6. washThe aqueous layer was washed with diethyl ether (3×20 mL)
  7. washThe combined organic layers were washed with brine (10 mL)
  8. dry with materialdried (Na2SO4)
  9. filtrationfiltered
  10. concentrationconcentrated under reduced pressure
  11. customThe crude product was purified on a 24 g SiO2 cartridge

出典と根拠

ORDレコード
ord-e638a892f4e34f2da1e1ed20d512a3bc
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09045461B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート