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

HRID 32602

反応式

HRID 32602 の反応式
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]

参加物

4

反応物 3

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

生成物 1

HCID 179658946-Iodopyrimidine-4,5-diamine収率 98%

反応条件

温度
0 °C

実験手順

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%);

後処理

  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

出典と根拠

ORDレコード
ord-36d650d9bef54b7e970ce0e95d3a1b3e
出典データセット
uspto-grants-2008_09
特許番号
US07427616B2

関連ノート

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