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Acetone → 4-Methoxy-4-(methoxymethyl)cyclohexanone

HRID 930960
ノート
印刷プレビュー

反応式

HRID 930960 の反応式
[CH3:1][O:2][C:3]1([CH2:13][O:14][CH3:15])[CH2:12][CH2:11][C:6]2(OCC[O:7]2)[CH2:5][CH2:4]1.CC(C)=O.O.CC1C=CC(S(O)(=O)=O)=CC=1>O>[CH3:1][O:2][C:3]1([CH2:13][O:14][CH3:15])[CH2:4][CH2:5][C:6](=[O:7])[CH2:11][CH2:12]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 180AcetoneHCID 521998p-Toluenesulfonic acid monohydrateHCID 712474008-Methoxy-8-(methoxymethyl)-1,4-dioxaspiro[4.5]decane

生成物 1

HCID 857431314-Methoxy-4-(methoxymethyl)cyclohexanone

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture comprising 217 g (1.00 mol) 8-methoxy-8-(methoxymethyl)-1,4-dioxaspiro[4.5]decane (prepared according to intermediate example 16e), 1.7 L acetone, 0.86 L water and 30.5 g 4-methylbenzenesulfonic acid hydrate was stirred at 23° C. overnight. The acetone was removed, 0.5 L saturated aqueous sodium hydrogencarbonate added followed by 0.4 L brine. The mixture was extracted with ethyl acetate, the combined organic layers were washed with brine and dried over sodium sulfate. After filtration and removal of the solvent 180 g (max. 100%) of the title compound were obtained that was used without further purification.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. customThe acetone was removed
  2. addition0.5 L saturated aqueous sodium hydrogencarbonate added
  3. extractionThe mixture was extracted with ethyl acetate
  4. washthe combined organic layers were washed with brine
  5. dry with materialdried over sodium sulfate
  6. filtrationAfter filtration and removal of the solvent 180 g (max. 100%) of the title compound
  7. customwere obtained
  8. customthat was used without further purification

出典と根拠

ORDレコード
ord-f7315733175b45699d7356835f2c2b5b
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09296757B2

反応ノート

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