Phenol, 4-(trans-4-propylcyclohexyl)- → HCID 178447904、化合物

HRID 323994

反応式

HRID 323994 の反応式
[CH2:1]([CH:4]1[CH2:9][CH2:8][CH:7]([C:10]2[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=2)[CH2:6][CH2:5]1)[CH2:2][CH3:3].[H][H]>C1(C)C=CC=CC=1.[Pd]>[CH2:1]([C@H:4]1[CH2:5][CH2:6][C@H:7]([CH:10]2[CH2:15][CH2:14][C:13](=[O:16])[CH2:12][CH2:11]2)[CH2:8][CH2:9]1)[CH2:2][CH3:3]

参加物

5

反応物 2

HCID 3126231Phenol, 4-(trans-4-propylcyclohexyl)-HCID 178418361HCID 178418361、化合物

生成物 1

HCID 178447904HCID 178447904、化合物収率 86%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 1140Toluene溶媒

反応条件

温度
50 °C

実験手順

A soluton of 500 g of 4-(4-n-propylcyclohexyl)-phenol in 5 l of toluene is hydrogenated at a hydrogen pressure of 5 bar and 120° C. in the presence of 50 g of palladium on activated carbon (5% by weight). The reaction mixture is filtered and freed from water by azeotropic distillation. It is then treated with 110 g of pyridine sulfone (pyridine-sulfur trioxide complex), stirred at 50° C. for 1 hour and filtered using basic alumina. After removal of the solvent, 433 g (86% yield) of the trans-4-(4-n-propylcyclohexyl)cyclohexanone remain as a colourless solidified melt having a purity of 99.5% (GC).

後処理

  1. filtrationThe reaction mixture is filtered
  2. distillationfreed from water by azeotropic distillation
  3. additionIt is then treated with 110 g of pyridine sulfone (pyridine-sulfur trioxide complex)
  4. filtrationfiltered

出典と根拠

ORDレコード
ord-4bebb5f1d5674eec986d2bae6365ab4b
出典データセット
uspto-grants-2001_04
特許番号
US06215028B1

関連ノート

読み込み中…