Water → HCID 178448077, 화합물

HRID 2254932노트

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HRID 2254932 반응식
[CH2:1]([CH:4]1[CH2:9][CH2:8][CH:7]([CH:10]([CH2:13][OH:14])[CH2:11][OH:12])[CH2:6][CH2:5]1)[CH2:2][CH3:3].[F:15][C:16]1[CH:17]=[C:18]([CH:21]=[CH:22][C:23]=1[F:24])[CH:19]=O.CC1C=CC(S(O)(=O)=O)=CC=1.O>ClCCl>[F:15][C:16]1[CH:17]=[C:18]([C@H:19]2[O:12][CH2:11][C@H:10]([C@H:7]3[CH2:8][CH2:9][C@H:4]([CH2:1][CH2:2][CH3:3])[CH2:5][CH2:6]3)[CH2:13][O:14]2)[CH:21]=[CH:22][C:23]=1[F:24]

참가 물질

6

반응물 4

HCID 962WaterHCID 6101p-Toluenesulfonic acidHCID 5880883,4-DifluorobenzaldehydeHCID 112294182-(4-Propylcyclohexyl)propane-1,3-diol

생성물 1

HCID 178448077HCID 178448077, 화합물수율 62.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

In 40 cm3 of dichloromethane, 1.5 g (0.008 mol) of 2-(4'-propylcyclohexyl)propane-1,3-diol, 1.5 g (0.01 mol) of 3,4-difluorobenzaldehyde (manufactured by Aldrich), and 0.1 g of TsOH were refluxed for 3 hours over a hot water bath fitted with a Dean-Stark trap and the water formed was removed continuously 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 1.6 g (0.005 mol) of trans-2-(3',4'-difluorophenyl)-5-(trans-4'-propylcyclohexyl)-1,3-dioxane. The phase transition points, measured by DSC, were: ##STR31## wherein C is the crystal phase, N is the nematic phase and I is the isotropic liquid phase.

후처리

  1. customfitted with a Dean-Stark trap
  2. customwas removed continuously 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-dfd4427bed2a4e64ad9bc63e058c39cc
출처 데이터셋
uspto-grants-1993_08
특허 번호
US05238599

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