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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Allyl iodide → HCID 68816871, 화합물

HRID 657080
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HRID 657080 반응식
[F:1][C:2]1[CH:3]=[N+:4]([O-:13])[C:5]2[CH:6]=[CH:7][C:8](=[O:12])[NH:9][C:10]=2[CH:11]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:20](I)[CH:21]=[CH2:22]>CN(C=O)C>[F:1][C:2]1[CH:3]=[N+:4]([O-:13])[C:5]2[CH:6]=[CH:7][C:8](=[O:12])[N:9]([CH2:22][CH:21]=[CH2:20])[C:10]=2[CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11166Allyl iodideHCID 11430Potassium CarbonateHCID 688164937-fluoro-1,5-naphthyridin-2(1H)-one 5-oxide

생성물 1

HCID 68816871HCID 68816871, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Crude 7-fluoro-1,5-naphthyridin-2(1H)-one 5-oxide (0.995 g, 5.524 mmol) and potassium carbonate were stirred in anhydrous DMF (20 mL) under argon, and allyl iodide (1.5 mL, ca. 3 eq.) was added. The mixture was stirred at rt overnight. The solvent was removed under reduced pressure and the residue was partitioned between DCM (100 mL) and water (50 mL). The organic phase was separated using a hydrophobic frit and the aqueous phase was extracted with DCM (2×50 mL). The combined organic extracts were dried over anhydrous sodium sulphate, filtered and evaporated under reduced pressure to give the crude product as a brown gum. This was purified by column chromatography on silica gel eluted with 0-10% methanol in DCM. Appropriate fractions were combined and evaporated under reduced pressure to give 7-fluoro-1-(2-propen-1-yl)-1,5-naphthyridin-2(1H)-one 5-oxide (0.341 g) as a tan amorphous solid.

후처리

  1. customThe solvent was removed under reduced pressure
  2. customthe residue was partitioned between DCM (100 mL) and water (50 mL)
  3. customThe organic phase was separated
  4. extractionthe aqueous phase was extracted with DCM (2×50 mL)
  5. dry with materialThe combined organic extracts were dried over anhydrous sodium sulphate
  6. filtrationfiltered
  7. customevaporated under reduced pressure
  8. customto give the crude product as a brown gum
  9. customThis was purified by column chromatography on silica gel
  10. washeluted with 0-10% methanol in DCM
  11. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-cc1ad70fedf34e5c8a48f2bfc63117f2
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08071592B2

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