2,4-DI-Tert-butylcyclohexanol → Cyclohexanone, 2,4-bis(1,1-dimethylethyl)-

HRID 477425

반응식

HRID 477425 반응식
[C:1]([CH:5]1[CH2:10][CH:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH2:8][CH2:7][CH:6]1[OH:15])([CH3:4])([CH3:3])[CH3:2]>[Cu].[Cr]>[C:1]([CH:5]1[CH2:10][CH:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH2:8][CH2:7][C:6]1=[O:15])([CH3:4])([CH3:3])[CH3:2]

참가 물질

3

반응물 1

HCID 5460322,4-DI-Tert-butylcyclohexanol

생성물 1

HCID 114442Cyclohexanone, 2,4-bis(1,1-dimethylethyl)-수율 97.7%

시약·촉매·용매 1

HCID 9833946Chromium, compd. with copper (1:1)촉매

실험 절차

200 g (0.944 mole) of the 2,4-di-tert-butylcyclohexanol as prepared in Synthetic Example 2 and 2.0 g of a copper/chromium catalyst were introduced into a 500 ml four-necked flask and vigorously stirred therein at a temperature of 215° to 220° C. under a reduced pressure of 200 to 300 mmHg. This dehydrogenation procedure was carried out for 15 hours. After completion of the reaction, the heating and stirring were ceased and the reaction mixture was cooled to room temperature. Then the catalyst was filtered off. Thus 194 g of crude 2,4-di-tert-butylcyclohexanone having a cis/trans ratio of 81/19 was obtained. This product was rectified under reduced pressure in a Helipack packing column of a number of theoretical plates of 5 to give 158 g of 2,4-di-tert-butylcyclohexanone (b.p.: 93° to 94° C./3 mm Hg). This product had a cis/trans ratio of 85/15.

후처리

  1. additionwere introduced into a 500 ml four-necked flask
  2. customat a temperature of 215° to 220° C.
  3. customAfter completion of the reaction
  4. stirringthe heating and stirring
  5. filtrationThen the catalyst was filtered off

출처 및 근거

ORD 기록
ord-c3df95391bc24c0ab6873c4f629bdb9a
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04888323

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