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Propylene Glycol → HCID 14880907, 화합물

HRID 359251
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HRID 359251 반응식
[C:1]([C:9]1[CH:10]=[N:11][C:12]([Cl:15])=[CH:13][CH:14]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:16](O)[CH:17]([OH:19])[CH3:18].B(F)(F)F.CCOCC.[OH-].[Na+]>C1(C)C=CC=CC=1>[Cl:15][C:12]1[N:11]=[CH:10][C:9]([C:1]2([C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[O:19][CH:17]([CH3:18])[CH2:16][O:8]2)=[CH:14][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 1030Propylene GlycolHCID 8000Boron trifluoride etherateHCID 14798Sodium HydroxideHCID 3061713Methanone, (6-chloro-3-pyridinyl)phenyl-

생성물 1

HCID 14880907HCID 14880907, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To 25 ml of a solution of 1.5 g of 3-benzoyl-6-chloropyridine and 3.2 g of 1,2-propanediol in toluene, 1.2 g of boron trifluoride etherate was added. The resulting mixture was heated under reflux for six hours while removing the water thus formed therefrom. Then the reaction mixture was cooled, poured into an aqueous solution of sodium hydroxide and extracted with ether. The organic phase was washed with water and dried over anhydrous sodium sulfate. After filtering off the sodium sulfate and distilling off the solvent in vacuo, 2-(6-chloropyridin-3-yl)-4-methyl-2-phenyl-1,3-dioxolane was obtained m.p.: 44°-51° C.

후처리

  1. temperatureThe resulting mixture was heated
  2. temperatureunder reflux for six hours
  3. customwhile removing the water
  4. customthus formed
  5. temperatureThen the reaction mixture was cooled
  6. extractionextracted with ether
  7. washThe organic phase was washed with water
  8. dry with materialdried over anhydrous sodium sulfate
  9. filtrationAfter filtering off the sodium sulfate
  10. distillationdistilling off the solvent in vacuo

출처 및 근거

ORD 기록
ord-54978bc34de84cb6b5eb9421afcbbcae
출처 데이터셋
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05000778

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