Selectfluor → 4-Chloro-5-fluoro-7H-pyrrolo(2,3-d)pyrimidine

HRID 2252710

반응식

HRID 2252710 반응식
C[Sn](C)(C)[C:3]1[C:11]2[C:10]([Cl:12])=[N:9][CH:8]=[N:7][C:6]=2[NH:5][CH:4]=1.[F:15][B-](F)(F)F.F[B-](F)(F)F.ClC[N+]12CC[N+](F)(CC1)CC2>CC#N>[F:15][C:3]1[C:11]2[C:10]([Cl:12])=[N:9][CH:8]=[N:7][C:6]=2[NH:5][CH:4]=1

참가 물질

4

반응물 2

HCID 2724933Selectfluor2회HCID 114612365-(Trimethylstannyl)-4-chloro-7H-pyrrolo[2,3-d]pyrimidine

생성물 1

HCID 113212244-Chloro-5-fluoro-7H-pyrrolo(2,3-d)pyrimidine

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of the compound from Step B (1.97 g, 6.20 mmol) in CH3CN (60 mL) was added [1-(chloromethyl)-4-fluoro-1,4-diazoniabicyclo[2.2.2]octane bis(tetrafluoroborate)] (SELECTFLUOR® fluorinating reagent) (2.40 g, 6.5 mmol) in one portion and the reaction mixture was stirred at room temperature for 7 h. The white precipitate was filtered off, and the filtrate was evaporated to dryness. The residue was purified over silica gel using ethyl acetate/hexane (3:7) as the eluent. Fractions containing the product were pooled and eveporated in vacuo to give the title compound as a colorless solid.

후처리

  1. filtrationThe white precipitate was filtered off
  2. customthe filtrate was evaporated to dryness
  3. customThe residue was purified over silica gel
  4. additionFractions containing the product

출처 및 근거

ORD 기록
ord-72b7a59eb3684225abb22ea91a3f91ee
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07323453B2

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