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

HRID 980826

반응식

HRID 980826 반응식
[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

참가 물질

4

반응물 1

HCID 750554-Cyclohexylresorcinol

생성물 1

HCID 202209951,3-Dioxo-6-cyclohexyl-cyclohexane수율 63.8%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 14798Sodium Hydroxide용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-8fdfe03ebbbd4228a8bde573678a33a8
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04639453

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