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Methyl 2'-fluoro-5'-(methyloxy)-2-(3,3,5,5-tetramethyl-1-cyclohexen-1-yl)-1,1'-biphenyl-4-carboxylate → Methyl 2'-fluoro-5'-(methyloxy)-2-(3,3,5,5-tetramethylcyclohexyl)-1,1'-biphenyl-4-carboxylate

HRID 1662494
ノート
印刷プレビュー

反応式

HRID 1662494 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[C:10]1[CH:15]=[CH:14][C:13]([C:16]([O:18][CH3:19])=[O:17])=[CH:12][C:11]=1[C:20]1[CH2:25][C:24]([CH3:27])([CH3:26])[CH2:23][C:22]([CH3:29])([CH3:28])[CH:21]=1>[Pt](=O)=O.CCOC(C)=O.CO>[F:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[C:10]1[CH:15]=[CH:14][C:13]([C:16]([O:18][CH3:19])=[O:17])=[CH:12][C:11]=1[CH:20]1[CH2:25][C:24]([CH3:27])([CH3:26])[CH2:23][C:22]([CH3:29])([CH3:28])[CH2:21]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 57706531Methyl 2'-fluoro-5'-(methyloxy)-2-(3,3,5,5-tetramethyl-1-cyclohexen-1-yl)-1,1'-biphenyl-4-carboxylate

生成物 1

HCID 57707074Methyl 2'-fluoro-5'-(methyloxy)-2-(3,3,5,5-tetramethylcyclohexyl)-1,1'-biphenyl-4-carboxylate収率 59.3%

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 21584119Ethylacetate methanol溶媒

実験手順

A screw-cap pressure tube was charged with 69.31B (0.22 g, 0.55 mmol), 1:1 EtOAc/MeOH (10 mL), and platinum(IV) oxide (0.025 g, 0.11 mmol). The tube was purged three times with H2 at 50 psi and sealed, and the contents were stirred overnight. The mixture was diluted with EtOAc, filtered through silica gel (EtOAc), and concentrated. The crude product was purified by silica gel flash chromatography (0-8% EtOAc/hexane) to afford 69.32A (0.13 g, 59% yield) as a colorless oil.

後処理

  1. customThe tube was purged three times with H2 at 50 psi
  2. customsealed
  3. additionThe mixture was diluted with EtOAc
  4. filtrationfiltered through silica gel (EtOAc)
  5. concentrationconcentrated
  6. customThe crude product was purified by silica gel flash chromatography (0-8% EtOAc/hexane)

出典と根拠

ORDレコード
ord-28a7a0c61e1f474ca8d54c5af823b32b
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08030354B2

反応ノート

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