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Selenium Dioxide → HCID 56598243, 화합물

HRID 1505467
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HRID 1505467 반응식
N[C:2]1[C:3]2[C:27]3(CCOC3)[C:26](=[O:32])[NH:25][C:4]=2[N:5]=[C:6]([C:8]2[C:16]3[C:11](=[N:12][CH:13]=[CH:14][CH:15]=3)[N:10]([CH2:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[F:24])[N:9]=2)[N:7]=1.[Se](=O)=[O:34]>O1CCOCC1>[F:24][C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=1[CH2:17][N:10]1[C:11]2=[N:12][CH:13]=[CH:14][CH:15]=[C:16]2[C:8]([C:6]2[N:7]=[CH:2][C:3]3[C:27](=[O:34])[C:26](=[O:32])[NH:25][C:4]=3[N:5]=2)=[N:9]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24007Selenium DioxideHCID 56598426HCID 56598426, 화합물

생성물 1

HCID 56598243HCID 56598243, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

2.00 g (5.550 mmol) of Example 4 were initially charged in dioxane (200 ml), 3.079 g (27.751 mmol) of selenium dioxide were added and the mixture was heated at reflux for 2 h. After cooling, the mixture was filtered and the filtrate was concentrated and purified by chromatography on silica gel (mobile phase:cyclohexane/ethyl acetate 1:1). This gave 890 mg of the title compound (42% of theory).

후처리

  1. temperature
the mixture was heated
  • temperatureat reflux for 2 h
  • temperatureAfter cooling
  • filtrationthe mixture was filtered
  • concentrationthe filtrate was concentrated
  • custompurified by chromatography on silica gel (mobile phase:cyclohexane/ethyl acetate 1:1)
  • 출처 및 근거

    ORD 기록
    ord-0391916ede6640368fdc5c07d56a0498
    출처 데이터셋
    uspto-grants-2015_12
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US09216978B2

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