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Water → HCID 178445641、化合物

HRID 2254946
ノート
印刷プレビュー

反応式

HRID 2254946 の反応式
[CH2:1]([CH:5]1[CH2:10][CH2:9][CH:8]([CH:11]([CH2:14][OH:15])[CH2:12][OH:13])[CH2:7][CH2:6]1)[CH2:2][CH2:3][CH3:4].[C:16]([C:18]1[CH:25]=[CH:24][C:21]([CH:22]=O)=[CH:20][CH:19]=1)#[N:17].CC1C=CC(S(O)(=O)=O)=CC=1.O>ClCCl>[C:16]([C:18]1[CH:25]=[CH:24][C:21]([C@H:22]2[O:13][CH2:12][C@H:11]([C@H:8]3[CH2:7][CH2:6][C@H:5]([CH2:1][CH2:2][CH2:3][CH3:4])[CH2:10][CH2:9]3)[CH2:14][O:15]2)=[CH:20][CH:19]=1)#[N:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 6101p-Toluenesulfonic acidHCID 660424-CyanobenzaldehydeHCID 404183872-(4-Butylcyclohexyl)propane-1,3-diol

生成物 1

HCID 178445641HCID 178445641、化合物収率 20%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

In dichloromethane, 4.6 g (0.02 mol) of 2-(4'-butylcyclohexyl) propane-1,3-diol, 3.2 g (0.024 mol) of 4-cyanobenzaldehyde, and 0.1 g of TsOH were refluxed for three hours over a hot water bath fitted with a Dean-Stark trap and the water formed was continuously removed from the reaction system. The reaction solution was washed with water and the dichloromethane was distilled off. The distillation residue was recrystallized from a solvent mixture of acetone and methanol to yield 1.1 g (0.004 mol) of trans-2-(4'-cyanophenyl)-5-(trans-4'-butylcyclohexyl)-1,3-dioxane. The phase transition points of this compound, measured by DSC, were: ##STR53##

後処理

  1. customfitted with a Dean-Stark trap
  2. customwas continuously removed from the reaction system
  3. washThe reaction solution was washed with water
  4. distillationthe dichloromethane was distilled off
  5. customThe distillation residue was recrystallized from a solvent mixture of acetone and methanol

出典と根拠

ORDレコード
ord-828954675cc8479facbe92a51c37c6e0
出典データセット
uspto-grants-1993_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05238599

反応ノート

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