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Water → 4-Methyl-2-(4,6,6-trimethyl-1-cyclohexen-1-yl)-1,3-dioxolan

HRID 566856
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HRID 566856 반응식
[CH3:1][CH:2]1[CH2:7][C:6]([CH3:9])([CH3:8])[C:5]([CH:10]=[O:11])=[CH:4][CH2:3]1.[CH2:12]([OH:16])[CH:13](O)[CH3:14].O>C1(C)C=CC=CC=1.C1(C)C=CC(S(O)(=O)=O)=CC=1>[CH3:14][CH:13]1[CH2:12][O:16][CH:10]([C:5]2[C:6]([CH3:8])([CH3:9])[CH2:7][CH:2]([CH3:1])[CH2:3][CH:4]=2)[O:11]1
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참가 물질

6

반응물 3

HCID 962WaterHCID 1030Propylene GlycolHCID 212637424,6,6-Trimethylcyclohex-1-ene-1-carbaldehyde

생성물 1

HCID 212637524-Methyl-2-(4,6,6-trimethyl-1-cyclohexen-1-yl)-1,3-dioxolan수율 65.1%

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매HCID 1140Toluene용매

실험 절차

4,6,6-Trimethyl-1-cyclohexen-1-carbaldehyde (2 g, 13 mmole), 1,2-propanediol (4 g, 53 mmole) and p-toluenesulfonic acid (50 mg) were refluxed in 20 ml of toluene, with water separation in a Dean-Stark apparatus, during 6 h. The resulting solution was washed with a NaHCO3 solution and the crude product distilled at a bath temperature of 80°/0.5 hPa, to obtain 1.78 g of the desired product in the form of a mixture of isomers.

후처리

  1. washThe resulting solution was washed with a NaHCO3 solution
  2. distillationthe crude product distilled at a bath temperature of 80°/0.5 hPa

출처 및 근거

ORD 기록
ord-6470f5e3c117442d98ad52d6a8e38a77
출처 데이터셋
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06177400B1

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