Water → HCID 20444150, 화합물

HRID 1632244노트

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HRID 1632244 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][O:10][C:11]2[CH:16]=[CH:15][C:14]([C:17](=[O:19])[CH3:18])=[CH:13][CH:12]=2)=[CH:5][CH:4]=1.O.[Se](=O)=[O:22]>O1CCOCC1>[OH2:2].[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:9][O:10][C:11]2[CH:12]=[CH:13][C:14]([C:17](=[O:19])[CH:18]=[O:22])=[CH:15][CH:16]=2)=[CH:7][CH:8]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 24007Selenium DioxideHCID 10377701Ethanone, 1-[4-[(4-methoxyphenyl)methoxy]phenyl]-

생성물 1

HCID 20444150HCID 20444150, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A 10.0 g portion of 1-[4-[(4-methoxyphenyl)-methoxy]phenyl]ethanone was dissolved in 50 ml of hot p-dioxane. A 2.0 ml portion of water and 4.4 g of selenium dioxide were added and the mixture was stirred at reflux for 67 hours, then cooled and filtered through diatomaceous earth. The filtrate was poured into 300 ml of water and the solid collected. This solid was extracted with eight 100 ml portions of ethyl acetate. The extracts were combined, washed with water, dried and evaporated. The residue was dissolved in 100 ml of boiling toluene, treated with charcoal and filtered through diatomaceous earth. The filtrate was treated with 200 ml. of hexane, giving the desired product as a pale yellow solid, m.p. 127°-138° C.

후처리

  1. temperatureat reflux for 67 hours
  2. temperaturecooled
  3. filtrationfiltered through diatomaceous earth
  4. additionThe filtrate was poured into 300 ml of water
  5. customthe solid collected
  6. extractionThis solid was extracted with eight 100 ml portions of ethyl acetate
  7. washwashed with water
  8. customdried
  9. customevaporated
  10. dissolutionThe residue was dissolved in 100 ml of boiling toluene
  11. additiontreated with charcoal
  12. filtrationfiltered through diatomaceous earth
  13. additionThe filtrate was treated with 200 ml

출처 및 근거

ORD 기록
ord-020bdd08cd31490a83f4e9284a26f9ba
출처 데이터셋
uspto-grants-1984_10
특허 번호
US04474809

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