Acetic Acid → 1-Methoxy-1,1'-bicyclohexane-4-one

HRID 1816764ノート

反応式

HRID 1816764 の反応式
[CH:1]1([C:7]2([O:17][CH3:18])[CH2:16][CH2:15][C:10]3(OCC[O:11]3)[CH2:9][CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(O)(=O)C.C(=O)([O-])O.[Na+].C(OCC)C>O>[CH3:18][O:17][C:7]1([CH:1]2[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]2)[CH2:16][CH2:15][C:10](=[O:11])[CH2:9][CH2:8]1

参加物

6

反応物 4

HCID 176Acetic AcidHCID 3283Diethyl EtherHCID 516892Sodium BicarbonateHCID 224947668-Cyclohexyl-8-methoxy-1,4-dioxaspiro[4.5]decane

生成物 1

HCID 224929241-Methoxy-1,1'-bicyclohexane-4-one収率 107.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 8-cyclohexyl-8-methoxy-1,4-dioxaspiro[4.5]decane (1.15 g) and acetic acid (40 ml) in water was stirred at 100° C. for 6 hours. After cooling to room temperature, the reaction mixture was added to a mixture of sodium hydrogen carbonate solution and diethyl ether. The organic layer was taken, washed with sodium hydrogen carbonate solution and dried over magnesium sulfate. The magnesium sulfate was filtered off, and the filtrate was concentrated under reduced pressure to give 1-methoxy-1,1′-bicyclohexane-4-one (1.018 g).

後処理

  1. washwashed with sodium hydrogen carbonate solution
  2. dry with materialdried over magnesium sulfate
  3. filtrationThe magnesium sulfate was filtered off
  4. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-b6fc3e30c9844efebb1d782acaae039c
出典データセット
uspto-grants-2005_04
特許番号
US06884868B1

反応ノート

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