4-Cyclohexylresorcinol → 1,3-Dioxo-6-cyclohexyl-cyclohexane

HRID 980826ノート

反応式

HRID 980826 の反応式
[CH:1]1([C:7]2[CH:13]=[CH:12][C:10]([OH:11])=[CH:9][C:8]=2[OH:14])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1>[OH-].[Na+].[Ni]>[O:14]=[C:8]1[CH:7]([CH:1]2[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]2)[CH2:13][CH2:12][C:10](=[O:11])[CH2:9]1

参加物

4

反応物 1

HCID 750554-Cyclohexylresorcinol

生成物 1

HCID 202209951,3-Dioxo-6-cyclohexyl-cyclohexane収率 63.8%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 14798Sodium Hydroxide溶媒

実験手順

20.0 g (0.104 mol) of 4-cyclohexylresorcinol are dissolved in 40 ml of ten percent strength sodium hydroxide solution and are hydrogenated in the presence of 5 g of Raney nickel in an autoclave at 90° under 20 bar for 5 hours. The reaction mixture is rinsed out of the autoclave with alcohol. After removal of the catalyst, 100 ml of 90 percent strength acetic acid are slowly added to the solution. After addition of water, the reaction product crystallises out. It is dried in vacuo over NaOH. 12.9 g of 1,3-dioxo-6-cyclohexyl-cyclohexane of melting point 137°-140° C. are obtained. After recrystallisation from ethyl acetate, the product has a melting point of 142°-144° C. (literature). Yield: 11.1 g (=55%).

後処理

  1. washThe reaction mixture is rinsed out of the autoclave with alcohol
  2. customAfter removal of the catalyst, 100 ml of 90 percent strength acetic acid
  3. additionare slowly added to the solution
  4. additionAfter addition of water
  5. customthe reaction product crystallises out
  6. dry with materialIt is dried in vacuo over NaOH

出典と根拠

ORDレコード
ord-8fdfe03ebbbd4228a8bde573678a33a8
出典データセット
uspto-grants-1987_01
特許番号
US04639453

反応ノート

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