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Sodium Hydroxide → 2,2,4,6,7-Pentamethyl-2,3-dihydrobenzofuran

HRID 1850370
ノート
印刷プレビュー

反応式

HRID 1850370 の反応式
[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([CH3:9])=[C:4]([CH2:10][C:11]([CH3:13])=[CH2:12])[C:3]=1[OH:14].O.C1(C)C=CC(S(O)(=O)=O)=CC=1.[OH-].[Na+]>C1(C)C=CC=CC=1>[CH3:12][C:11]1([CH3:13])[CH2:10][C:4]2[C:5]([CH3:9])=[CH:6][C:7]([CH3:8])=[C:2]([CH3:1])[C:3]=2[O:14]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 521998p-Toluenesulfonic acid monohydrateHCID 10655310Phenol, 2,3,5-trimethyl-6-(2-methyl-2-propenyl)-

生成物 1

HCID 117454372,2,4,6,7-Pentamethyl-2,3-dihydrobenzofuran収率 85.4%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 2,3,5-trimethyl-6-(2-methylprop-2-en-1-yl)phenol (13.0 g, 68.3 mmol) synthesized in Reference Example 2, p-toluenesulfonic acid monohydrate (1.30 g, 6.83 mmol) and toluene (130 mL) was stirred under heated reflux for 1.5 hours. After cooled to room temperature, the reaction solution was distributed by addition of 1N sodium hydroxide aqueous solution. The organic layer was washed with 1N sodium hydroxide aqueous solution and saturated saline, and then dried using anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the obtained residue was purified by basic silica gel chromatography (hexane-ethyl acetate 49:1 to 24:1) to give 11.1 g of the title compound (yield: 85%).

後処理

  1. temperatureunder heated
  2. temperaturereflux for 1.5 hours
  3. washThe organic layer was washed with 1N sodium hydroxide aqueous solution and saturated saline
  4. customdried
  5. customThe solvent was removed under reduced pressure
  6. customthe obtained residue was purified by basic silica gel chromatography (hexane-ethyl acetate 49:1 to 24:1)

出典と根拠

ORDレコード
ord-47396749364f4795854d7b5966adcde1
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08957069B2

反応ノート

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