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2-Aminophenol → 3-[2-(Benzoxazol-2-yl)ethenyl]-5-ethyl-6-benzyloxymethyl-2-benzyloxypyridine

HRID 2081536
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HRID 2081536 반응식
[Cl-].[O:2]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[N:4]=[C:3]1[CH2:11][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.NC1C=CC=CC=1O.CC1C=CC(C)=C(N)C=1O.[H-].[Na+].[CH2:51]([O:58][C:59]1[N:66]=[C:65]([CH2:67][O:68][CH2:69][C:70]2[CH:75]=[CH:74][CH:73]=[CH:72][CH:71]=2)[C:64]([CH2:76][CH3:77])=[CH:63][C:60]=1[CH:61]=O)[C:52]1[CH:57]=[CH:56][CH:55]=[CH:54][CH:53]=1>O1CCCC1.C(O)(=O)C>[O:2]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[N:4]=[C:3]1[CH:11]=[CH:61][C:60]1[C:59]([O:58][CH2:51][C:52]2[CH:53]=[CH:54][CH:55]=[CH:56][CH:57]=2)=[N:66][C:65]([CH2:67][O:68][CH2:69][C:70]2[CH:71]=[CH:72][CH:73]=[CH:74][CH:75]=2)=[C:64]([CH2:76][CH3:77])[CH:63]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 58012-AminophenolHCID 24758Sodium hydrideHCID 150363212-Amino-3,6-dimethylphenolHCID 19769114[(1,3-Benzoxazol-2-yl)methyl](triphenyl)phosphanium chlorideHCID 197691192-Benzyloxy-5-ethyl-6-benzyloxymethylnicotinaldehyde

생성물 1

HCID 67854280
3-[2-(Benzoxazol-2-yl)ethenyl]-5-ethyl-6-benzyloxymethyl-2-benzyloxypyridine

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 8028Tetrahydrofuran용매2회

실험 절차

To a suspension of [(benzoxazol-2-yl)methyl]triphenylphosphonium chloride (1.77 g, 4.12 mmol) (prepared using substantially the same procedures described in Example 5, but substituting 2-aminophenol and the intermediate thereof for the 2,5-dimethyl-6-aminophenol and its corresponding intermediate used therein), in dry tetrahydrofuran (20 mL), under a nitrogen atmosphere, was added 60% NaH/mineral oil (0.42 g, 10 mmol). After 0.5 hour a solution of 2-benzyloxy-5-ethyl-6-benzyloxymethylnicotinaldehyde (1.44 g, 4.0 mmol) in tetrahydrofuran (10 mL) was added and the reaction mixture was refluxed for 23 hours. The reaction was cooled, neutralized with acetic acid and partitioned between water and chloroform. The chloroform layer was washed with NaHCO3 solution, dried, filtered through a pad of charcoal and evaporated. This material was dissolved in chloroform and flash chromatographed through silica gel to give pure product as a yellow oil. The product was a mixture of cis and trans olefins.

후처리

  1. customprepared
  2. temperaturethe reaction mixture was refluxed for 23 hours
  3. temperatureThe reaction was cooled
  4. custompartitioned between water and chloroform
  5. washThe chloroform layer was washed with NaHCO3 solution
  6. customdried
  7. filtrationfiltered through a pad of charcoal
  8. customevaporated
  9. dissolutionThis material was dissolved in chloroform
  10. customflash chromatographed through silica gel
  11. customto give pure product as a yellow oil

출처 및 근거

ORD 기록
ord-f2aca578e4294c438761801cb74a803b
출처 데이터셋
uspto-grants-1993_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05185251

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