1,2-Butanediol → 2-tert-Butylcyclohexyloxybutanol

HRID 1757684

反応式

HRID 1757684 の反応式
[C:1]([CH:5]1[CH2:16][CH2:15][CH2:14][CH2:13][C:6]21[O:10][CH:9]([CH2:11][CH3:12])[CH2:8][O:7]2)([CH3:4])([CH3:3])[CH3:2].C(C1CCCCC1=O)(C)(C)C.C(O)C(O)CC>[Pd].C(O)(C)C>[C:1]([CH:5]1[CH2:16][CH2:15][CH2:14][CH2:13][CH:6]1[O:7][CH2:8][CH:9]([OH:10])[CH2:11][CH3:12])([CH3:4])([CH3:3])[CH3:2]

参加物

6

反応物 3

HCID 114291,2-ButanediolHCID 1026812-tert-ButylcyclohexanoneHCID 157895866-t-Butyl-2-ethyl-1,4-dioxaspiro[4.5]decane

生成物 1

HCID 1644222-tert-Butylcyclohexyloxybutanol収率 81.5%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 3776Isopropanol溶媒

実験手順

A 500 ml capacity autoclave was charged with 30 g (0.13 mol) of 6-t-butyl-2-ethyl-1,4-dioxaspiro[4.5]decane which has been prepared from 2-t-butylcyclohexanone and 1,2-butanediol, 150 g of isopropanol and 0.3 g of a catalyst of 5% palladium supported on active carbon (pH=7.6). The reaction was carried out under a hydrogen pressure of 70 kg/cm2 and at a temperature of 190° C. for 20 hours until completion of the absorption of hydrogen. After the reaction, the catalyst was removed by filtration and the resulting filtrate was subjected to distillation to obtain 24.2 g of 1-(2-t-butylcyclohexyloxy)-2-butanol (b.p.=122° to123° C./5 mmHg; yield=80%; cis:trans=66:34).

後処理

  1. customat a temperature of 190° C. for 20 hours until completion of the absorption of hydrogen
  2. customAfter the reaction
  3. customthe catalyst was removed by filtration
  4. distillationthe resulting filtrate was subjected to distillation

出典と根拠

ORDレコード
ord-32c3b9562e9942f6a1f53283c829a1d7
出典データセット
uspto-grants-1995_08
特許番号
US05446208

関連ノート

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