Hydrogen iodide → 6-Iodopyrimidine-4,5-diamine

HRID 32602

반응식

HRID 32602 반응식
Cl[C:2]1[N:7]=[CH:6][N:5]=[C:4]([NH2:8])[C:3]=1[NH2:9].[IH:10].C([O-])(O)=O.[Na+]>>[I:10][C:2]1[N:7]=[CH:6][N:5]=[C:4]([NH2:8])[C:3]=1[NH2:9]

참가 물질

4

반응물 3

HCID 24841Hydrogen iodideHCID 780104,5-Pyrimidinediamine, 6-chloro-2회HCID 516892Sodium Bicarbonate

생성물 1

HCID 179658946-Iodopyrimidine-4,5-diamine수율 98%

반응 조건

온도
0 °C

실험 절차

6-Chloropyrimidine-4,5-diamine (Intermediate 88) (90 mg) was added slowly to HI (57%, aq) (2 mL) at 0° C. The reaction mixture was allowed to stir at 0° C. for 30 minutes and then at ambient temperature for 24 hours. NaHCO3 (sat aq.) was added dropwise until the reaction mixture was pH 8. The product was extracted with EtOAc (3×15 mL). The combined organics were dried (MgSO4), filtered and concentrated in vacuo to afford the title compound as a grey solid (144 mg, 98%);

후처리

  1. waitat ambient temperature for 24 hours
  2. extractionThe product was extracted with EtOAc (3×15 mL)
  3. dry with materialThe combined organics were dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-36d650d9bef54b7e970ce0e95d3a1b3e
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07427616B2

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