反应详情

To a solution of THF (150 mL) was added ethyl 4-aminopyrrolo[2,1-f][1,2,4]triazine-6-carboxylate (2.29 g, 4.65 mmol) followed by 1 M DIBAL in THF (28.8 mL, 28.8 mmol). The solution was stirred at rt for 1 h. The rxn mixture was treated with EtOAc followed by aq Rochelle's salt. This heterogeneous mixture was then heated at 60° C. for 30 min. The solution was transferred to a separatory funnel, separated and washed with water. The aq layer was back extracted with EtOAc. The organic layer was dried (MgSO4), filtered, and concentrated to yield 550 mg (93%) of the desired product. MS [M+H]+=165; LCMS RT=1.03.

1. temperatureThis heterogeneous mixture was then heated at 60° C. for 30 min
2. customThe solution was transferred to a separatory funnel
3. customseparated
4. washwashed with water
5. extractionThe aq layer was back extracted with EtOAc
6. dry with materialThe organic layer was dried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated