HCID 18364408, 화합물 → HCID 17820729, 화합물

HRID 380241노트

반응식

HRID 380241 반응식
[Cl:1][C:2]1[C:3]2[CH:12]=[C:11]3[O:13][CH2:14][O:15][C:10]3=[CH:9][C:4]=2[S:5][C:6]=1[CH2:7][OH:8]>O1CCOCC1.C(OCC)(=O)C.O=[Mn]=O>[Cl:1][C:2]1[C:3]2[CH:12]=[C:11]3[O:13][CH2:14][O:15][C:10]3=[CH:9][C:4]=2[S:5][C:6]=1[CH:7]=[O:8]

참가 물질

5

반응물 1

HCID 18364408HCID 18364408, 화합물

생성물 1

HCID 17820729HCID 17820729, 화합물

시약·촉매·용매 3

HCID 14801Manganese dioxide촉매HCID 8857Ethyl Acetate용매HCID 312751,4-Dioxane용매

실험 절차

3.5 equivalents of MnO2 are added at ambient temperature under an inert atmosphere to a suspension of 0.12 mol of the compound obtained in Step C in 925 ml of anhydrous dioxane. After 3.5 hours' reaction at reflux, the reaction mixture is filtered while hot over Celite and rinsed with dioxane; the filtrate is then concentrated under reduced pressure. The residue obtained is taken up in 100 ml of ethyl acetate and the solution obtained is refluxed and then returned to ambient temperature. A precipitate forms, which is filtered off, rinsed with ethyl acetate and then with water and pentane, and finally dried in vacuo, allowing the expecting product to be isolated.

후처리

  1. customAfter 3.5 hours' reaction
  2. temperatureat reflux
  3. filtrationthe reaction mixture is filtered while hot over Celite
  4. washrinsed with dioxane
  5. concentrationthe filtrate is then concentrated under reduced pressure
  6. customThe residue obtained
  7. customthe solution obtained
  8. temperatureis refluxed
  9. customreturned to ambient temperature
  10. filtrationA precipitate forms, which is filtered off
  11. washrinsed with ethyl acetate
  12. dry with materialwith water and pentane, and finally dried in vacuo
  13. customto be isolated

출처 및 근거

ORD 기록
ord-8896757702694271ad44b325e5947096
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06302837B1

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