反応 #48373

反応方程式

HCl

3-azido-5-fluoropyridin-2-amine

Carbonate

→

title compound

収率 92.8%

5-Fluoropyridine-2,3-diamine

収率 92.8%

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   ろ過the mixture was filtered
2. 2
   洗浄rinsed with more tetrahydrofuran
3. 3
   濃縮concentrated
4. 4
   workup.DISSOLUTIONThis residue was dissolved in ethanol (50 mL)
5. 5
   その他purged with argon, and 10% palladium on carbon
6. 6
   workup.ADDITIONwas added (0.15 g)
7. 7
   workup.ADDITIONHydrogen was introduced (1 atm)
8. 8
   ろ過The catalyst was filtered
9. 9
   その他the solvent evaporated from the filtrate

実験手順

The HCl salt of 3-azido-5-fluoropyridin-2-amine (1.90 g, 10.0 mmol) was dissolved in tetrahydrofuran (100 mL) and treated with MP-Carbonate (Argonaut, 11.5 g). After 1 h, the mixture was filtered, rinsed with more tetrahydrofuran, and concentrated. This residue was dissolved in ethanol (50 mL), purged with argon, and 10% palladium on carbon was added (0.15 g). Hydrogen was introduced (1 atm) and the reaction stirred until complete. The catalyst was filtered and the solvent evaporated from the filtrate to give the title compound (1.18 g). MS 128.0 (M+1)

出典