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1-Bromooctane → 5-Ethoxy-2-(4-octyloxyphenyl)pyrimidine

HRID 330220
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HRID 330220 반응식
[CH2:1]([O:3][C:4]1[CH:5]=[N:6][C:7]([C:10]2[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=2)=[N:8][CH:9]=1)[CH3:2].[OH-].[K+].[CH2:19](Br)[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26]>C(O)C>[CH2:1]([O:3][C:4]1[CH:9]=[N:8][C:7]([C:10]2[CH:15]=[CH:14][C:13]([O:16][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])=[CH:12][CH:11]=2)=[N:6][CH:5]=1)[CH3:2]
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참가 물질

5

반응물 3

HCID 81401-BromooctaneHCID 14797Potassium HydroxideHCID 1358116944-(5-Ethoxypyrimidin-2-yl)phenol

생성물 1

HCID 144963945-Ethoxy-2-(4-octyloxyphenyl)pyrimidine수율 77.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 5-ethoxy-2-(4-hydroxyphenyl)pyrimidine (40 g) dissolved in ethanol (340 ml) were added potassium hydroxide (11.2 g) and octyl bromide (35.8 g), followed by keeping the mixture under reflux for 3 hours, distilling off ethanol (about 300 ml), extracting the residue with toluene (500 ml), washing the resulting organic layer with 2N--NaOH aqueous solution, further washing with water until the washing water became neutral, distilling off low boiling substances in the organic layer and recrystallizing the residue from ethanol to obtain 5-ethoxy-2-(4-octyloxyphenyl)pyrimidine (46.9 g). This product exhibited a phase transition of ##STR11##

후처리

  1. temperatureunder reflux for 3 hours
  2. distillationdistilling off ethanol (about 300 ml)
  3. extractionextracting the residue with toluene (500 ml)
  4. washwashing the resulting organic layer with 2N
  5. washNaOH aqueous solution, further washing with water until the washing water
  6. distillationdistilling off low boiling substances in the organic layer
  7. customrecrystallizing the residue from ethanol

출처 및 근거

ORD 기록
ord-d205f5953700432aa0beba22110c4900
출처 데이터셋
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04895671

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