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

HRID 477425

反応式

HRID 477425 の反応式
[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]

参加物

3

反応物 1

HCID 5460322,4-DI-Tert-butylcyclohexanol

生成物 1

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

試薬・触媒・溶媒 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c3df95391bc24c0ab6873c4f629bdb9a
出典データセット
uspto-grants-1989_12
特許番号
US04888323

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