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

HRID 2252710

反応式

HRID 2252710 の反応式
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

参加物

4

反応物 2

HCID 2724933Selectfluor2 回HCID 114612365-(Trimethylstannyl)-4-chloro-7H-pyrrolo[2,3-d]pyrimidine

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-72b7a59eb3684225abb22ea91a3f91ee
出典データセット
uspto-grants-2008_01
特許番号
US07323453B2

関連ノート

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