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Dimethylformamide → HCID 87780782, 화합물

HRID 2115155
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HRID 2115155 반응식
[Br:1][C:2]1[CH:7]=[C:6]([CH:8]2[CH2:13][CH2:12][CH:11]([CH:14]3[CH2:19][CH2:18][CH:17]([CH2:20][CH2:21][CH3:22])[CH2:16][CH2:15]3)[CH2:10][CH2:9]2)[CH:5]=[CH:4][C:3]=1O.[C:24](=[O:27])([O-])[O-].[K+].[K+].[CH2:30](Cl)[C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1.CN(C=O)C>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.O>[Br:1][C:2]1[CH:7]=[C:6]([CH:8]2[CH2:9][CH2:10][CH:11]([CH:14]3[CH2:15][CH2:16][CH:17]([CH2:20][CH2:21][CH3:22])[CH2:18][CH2:19]3)[CH2:12][CH2:13]2)[CH:5]=[CH:4][C:3]=1[CH:30]([O:27][CH:24]([C:3]1[CH:4]=[CH:5][C:6]([CH:8]2[CH2:9][CH2:10][CH:11]([CH:14]3[CH2:19][CH2:18][CH:17]([CH2:20][CH2:21][CH3:22])[CH2:16][CH2:15]3)[CH2:12][CH2:13]2)=[CH:7][C:2]=1[Br:1])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 7503Benzyl ChlorideHCID 11430Potassium CarbonateHCID 69316420HCID 69316420, 화합물

생성물 1

HCID 87780782HCID 87780782, 화합물수율 148.3%

시약·촉매·용매 2

HCID 74236Tetrabutylammonium Bromide
촉매
HCID 962Water용매

실험 절차

The foregoing 2-bromo-4-(4-(4-propylcyclohexyl)cyclohexyl)phenol (250 mg), potassium carbonate (109 mg), and benzyl chloride (135 mg) were mixed, to which were then added DMF (2 ml) and tetrabutylammonium bromide (20 mg), and the mixture was refluxed by heating for 30 minutes. After completion of the reaction, the reaction mixture was added in water and extracted with toluene. The resulting toluene layer was washed with water, rinsed with a sodium hydrogencarbonate aqueous solution, and then dried over anhydrous magnesium sulfate. The solution was concentrated in vacuo and then subjected to isolation and purification by silica gel column chromatography, thereby obtaining a colorless crystal (300 mg) of 2-bromo-4-(4-(4-propylcyclohexyl)cyclohexyl)phenylbenzyl ether.

후처리

  1. temperatureby heating for 30 minutes
  2. customAfter completion of the reaction
  3. extractionextracted with toluene
  4. washThe resulting toluene layer was washed with water
  5. washrinsed with a sodium hydrogencarbonate aqueous solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationThe solution was concentrated in vacuo
  8. customsubjected to isolation and purification by silica gel column chromatography

출처 및 근거

ORD 기록
ord-a4e77ca5034c483db80591e1a6a67b86
출처 데이터셋
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07435455B2

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