3,5-Dimethyl-1-(carbethoxymethylene)cyclohexane → Ethyl 3,5-dimethyl-cyclohexylacetate

HRID 1461953ノート

反応式

HRID 1461953 の反応式
[CH3:1][CH:2]1[CH2:7][CH:6]([CH3:8])[CH2:5][C:4](=[CH:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH2:3]1>[Ni].CO>[CH3:1][CH:2]1[CH2:7][CH:6]([CH3:8])[CH2:5][CH:4]([CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH2:3]1

参加物

4

反応物 1

HCID 146168253,5-Dimethyl-1-(carbethoxymethylene)cyclohexane

生成物 1

HCID 20454256Ethyl 3,5-dimethyl-cyclohexylacetate収率 98%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

実験手順

To a 1 liter autoclave which is fitted with heating means, cooling means and a stirrer are added 54 g of ethyl 3,5-dimethyl-cyclohexylideneacetate, 200 ml of absolute methanol and 3 g of Raney-nickel, which has been washed three times with absolute methanol. The mixture is hydrogenated at 100° C. under a hydrogen pressure of 40 atmospheres. The hydrogen uptake stops after 8 hours. The catalyst is filtered off, the filtrate is concentrated and the residue is distilled. There are obtained 52.3 g of ethyl 3,5-dimethyl-cyclohexylacetate.

後処理

  1. customTo a 1 liter autoclave which is fitted with heating means
  2. temperaturecooling means and a stirrer
  3. washhas been washed three times with absolute methanol
  4. customis hydrogenated at 100° C. under a hydrogen
  5. filtrationThe catalyst is filtered off
  6. concentrationthe filtrate is concentrated
  7. distillationthe residue is distilled

出典と根拠

ORDレコード
ord-4173557b978d467397387dd106b378f0
出典データセット
uspto-grants-1984_07
特許番号
US04457862

反応ノート

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