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Water → HCID 178445641, 화합물

HRID 2254946
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HRID 2254946 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

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

생성물 1

HCID 178445641HCID 178445641, 화합물수율 20%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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##

후처리

  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

출처 및 근거

ORD 기록
ord-828954675cc8479facbe92a51c37c6e0
출처 데이터셋
uspto-grants-1993_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05238599

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