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2-Methoxypropene → (Z)-2-(4,5-difluoro-2-hydroxybenzoyl)-3-hydroxypyridine O-t-butyloxime

HRID 862093
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HRID 862093 반응식
Br[C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[CH:4][C:3]=1[OH:10].C[O:12][C:13]([CH3:15])=[CH2:14].[CH3:16]CCCCC.[CH2:22]([Li])CCC.[C:27]([C:29]1[C:34]([O:35][Si](C)(C)C)=[CH:33][CH:32]=[CH:31][N:30]=1)#[N:28]>C(OCC)C>[C:13]([O:12]/[N:28]=[C:27](\[C:29]1[C:34]([OH:35])=[CH:33][CH:32]=[CH:31][N:30]=1)/[C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[CH:4][C:3]=1[OH:10])([CH3:15])([CH3:16])[CH3:14].[C:13]([O:12]/[N:28]=[C:27](/[C:29]1[C:34]([OH:35])=[CH:33][CH:32]=[CH:31][N:30]=1)\[C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[CH:4][C:3]=1[OH:10])([CH3:15])([CH3:22])[CH3:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 83002-MethoxypropeneHCID 27362882-Bromo-4,5-difluorophenolHCID 158191802-Cyano-3-trimethylsilyloxypyridineHCID 178418244HCID 178418244, 화합물

생성물 2

HCID 136395970(Z)-2-(4,5-difluoro-2-hydroxybenzoyl)-3-hydroxypyridine O-t-butyloximeHCID 136395971
(E)-2-(4,5-difluoro-2-hydroxybenzoyl)-3-hydroxypyridine O-t-butyloxime

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A mixture of 2-bromo-4,5-difluorophenol (7.27 g) and 2-methoxypropene (10 ml) was stirred for one hour at room temperature, followed by adding diethyl ether (75 ml) and cooling to -78° C. To the mixture was added dropwise, under argon atmosphere, a 1.6M solution of n-butyl lithium hexane solution (25 ml), followed by stirring for one hour. To the reaction mixture was then added dropwise 2-cyano-3-trimethylsilyloxypyridine (7.01 g). The cooling bath was removed, and the mixture was stirred for 3 hours while warming up to room temperature. To the reaction mixture was added ethanol (10 ml) to quench the reaction. The solvent was distilled off under reduced pressure. To the residue were added triethylamine (20 ml), O-t-butylhydroxylamine hydrochloride (3.06 g) and ethanol (50 ml). The mixture was heated for 5 hours under reflux. The solvent was distilled off. To the residue were added chloroform and water for extraction. The organic layer was dried (anhydrous magnesium sulfate), and the solvent was distilled off under reduced pressure. The residue was purified by means of a silica gel column chromatography (eluted with ethyl acetate/hexane) to give (Z)-2-(4,5-difluoro-2-hydroxybenzoyl)-3-hydroxypyridine O-t-butyloxime (5.19 g) and (E)-2-(4,5-difluoro-2-hydroxybenzoyl)-3-hydroxypyridine O-t-butyloxime (1.49 g) (Compounds 34 and 35).

후처리

  1. temperaturecooling to -78° C
  2. additionTo the mixture was added dropwise, under argon atmosphere
  3. stirringby stirring for one hour
  4. customThe cooling bath was removed
  5. stirringthe mixture was stirred for 3 hours
  6. temperaturewhile warming up to room temperature
  7. additionTo the reaction mixture was added ethanol (10 ml)
  8. customto quench
  9. customthe reaction
  10. distillationThe solvent was distilled off under reduced pressure
  11. additionTo the residue were added triethylamine (20 ml), O-t-butylhydroxylamine hydrochloride (3.06 g) and ethanol (50 ml)
  12. temperatureThe mixture was heated for 5 hours
  13. temperatureunder reflux
  14. distillationThe solvent was distilled off
  15. additionTo the residue were added chloroform and water
  16. extractionfor extraction
  17. dry with materialThe organic layer was dried (anhydrous magnesium sulfate)
  18. distillationthe solvent was distilled off under reduced pressure
  19. customThe residue was purified by means of a silica gel column chromatography (eluted with ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-f23239cda109476a9e87f261484308a8
출처 데이터셋
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05716971

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