3-Cyclopentene-1-acetaldehyde, 2,2,3-trimethyl- → 2,2,3-Trimethylcyclopentaneacetaldehyde

HRID 1975630ノート

反応式

HRID 1975630 の反応式
[CH3:1][C:2]1[C:6]([CH3:8])([CH3:7])[CH:5]([CH2:9][CH:10]=[O:11])[CH2:4][CH:3]=1.[H][H]>[Pd]>[CH3:8][C:6]1([CH3:7])[CH:2]([CH3:1])[CH2:3][CH2:4][CH:5]1[CH2:9][CH:10]=[O:11]

参加物

4

反応物 2

HCID 984973-Cyclopentene-1-acetaldehyde, 2,2,3-trimethyl-HCID 178418361HCID 178418361、化合物

生成物 1

HCID 224142552,2,3-Trimethylcyclopentaneacetaldehyde収率 90.7%

試薬・触媒・溶媒 1

HCID 23938Palladium触媒

反応条件

温度
80 °C

実験手順

A three liter autoclave with a stirrer is charged with 830 g of campholenic aldehyde and 56 g of catalyst Pd(5%)/C. Hydrogen is introduced until the pressure reaches 30 bars. The mixture is heated up to 80° C. with stirring for five hours. The calculated amount of hydrogen is now absorbed. The catalyst is separated by filtration and washed with ethanol. The solvent is removed by vacuum evaporation and 815 g of crude saturated aldehyde are obtained (purity: 95%, GC). The vacuum distillation of the crude through a Widmer column gives 763 g of pure product (purity 95%); bp20 85° C.; nD20 : 1,4553;

後処理

  1. customThe calculated amount of hydrogen is now absorbed
  2. customThe catalyst is separated by filtration
  3. washwashed with ethanol
  4. customThe solvent is removed by vacuum evaporation and 815 g of crude saturated aldehyde
  5. customare obtained (purity: 95%, GC)
  6. distillationThe vacuum distillation of the crude through a Widmer column

出典と根拠

ORDレコード
ord-09c1fcba6c654e019dc94b973e7802a6
出典データセット
uspto-grants-1994_02
特許番号
US05288701

反応ノート

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