反応 #60880

反応方程式

NaHCO3

6-Chloropyrimidine-4,5-diamine

Intermediate 88

6-Chloropyrimidine-4,5-diamine

HI

→

title compound

収率 98.0%

6-Iodopyrimidine-4,5-diamine

収率 98.0%

反応条件

後処理

1. 1
   workup.WAITat ambient temperature for 24 hours
2. 2
   抽出The product was extracted with EtOAc (3×15 mL)
3. 3
   乾燥The combined organics were dried (MgSO4)
4. 4
   ろ過filtered
5. 5
   濃縮concentrated in vacuo

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%);

出典