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HCID 14851960, 화합물 → 6(5H)-Phenanthridinone

HRID 1032784
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HRID 1032784 반응식
Cl[C:2]1[CH:3]=[CH:4][C:5]2[C:6]3[C:11]([C:12](=[O:19])[N:13](CC#C)[C:14]=2[CH:15]=1)=[CH:10][C:9](Cl)=[CH:8][CH:7]=3>O1CCCC1.CCCCCC>[CH:4]1[C:5]2[C:6]3[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=3)[C:12](=[O:19])[NH:13][C:14]=2[CH:15]=[CH:2][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 14851960HCID 14851960, 화합물

생성물 1

HCID 18536(5H)-Phenanthridinone

시약·촉매·용매 1

HCID 21883165Tetrahydrofuran hexane용매

실험 절차

The title compound was prepared by reacting 4-(2-chlorophenyl)-2-iodo-9-methyl-6H-thieno[3,2-f]1,2,4]triazolo[4,3-a][1,4]diazepine with 3.8-dichloro 5-(2-propynyl)-6(5H)-phenanthridinone under the conditions used in Example 37, but at the end, the reaction mixture was heated for minutes at 90°-95°. The product was isolated by chromatography over the 50-fold amount of silica gel using tetrahydrofuran/hexane 4:1 for elution. Crystallization of the combined clean fractions from tetrahydrofuran/ethyl acetate gave colorless crystals of 3,8-dichloro-5-{3-[4-(2-chlorophenyl)-9-methyl-6H-thieno[3,2-f][1,2,4]triazolo[4,3-a]1,4]diazepin-2-yl]-2-propynyl}-6(5H)-phenanthridinone with m.p. 218°-220°.

후처리

  1. temperatureat the end, the reaction mixture was heated for minutes at 90°-95°
  • customThe product was isolated by chromatography over the 50-fold amount of silica gel
  • washfor elution
  • customCrystallization of the combined clean fractions from tetrahydrofuran/ethyl acetate
  • 출처 및 근거

    ORD 기록
    ord-16dbb45c6a384799a429f4404e120713
    출처 데이터셋
    uspto-grants-1990_09
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04959361

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