Formic Acid → HCID 178427955, 화합물

반응식

Cl.[Cl:2][C:3]1[C:4]([CH3:11])=[C:5]([NH2:10])[C:6]([NH2:9])=[N:7][CH:8]=1.[CH:12](O)=O.[OH-].[Na+]>P(=O)(O)(O)O>[Cl:2][C:3]1[C:4]([CH3:11])=[C:5]2[N:10]=[CH:12][NH:9][C:6]2=[N:7][CH:8]=1

참가 물질

반응 조건

온도: 130 °C

실험 절차

The material from Step 2 (1 g) was dissolved in phosphoric acid (20 ml), then added to formic acid (10 ml) and heated (130° C.) for 1 h, and then cooled to RT for 3 d. The reaction mixture was then poured into ice (200 g) and the pH adjusted with 30% (w/v) aq. NaOH until solids formed. The solids were removed via filtration and rinsed with water. The filtrate (aqueous) was concentrated to dryness and extracted with hot EtOH repeatedly. The EtOH extracts were combined and concentrated to solids (3 g). The solids were extracted with hot MeCN (4×80 ml); the combined MeCN extracts were cooled to RT and solids precipitated. The precipitates were filtered (Celite) and the filtrate was concentrated to yield 6-chloro-7-methyl-3H-imidazo[4,5-b]pyridine (0.278 g). MS (ESI+) for m/z 168 (M+H)+.