HRID1801489
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
To a solution of 6,11-dihydro-5H-dipyrido[2,3-b:4′,3′-f]azepin-5-one (as described in WO 2007038215) (0.38 g) and dimethylformamide dimethylacetal (1.5 mL) in tetrahydrofuran (10 mL) were heated at 60° C. under nitrogen for 24 hours. Additional dimethylformamide dimethylacetal (2 mL) was then added and the mixture heated at 60° C. under nitrogen for an additional 48 hours. The reaction mixture was cooled and solvent removed under reduced pressure to give the desired product, (E)-6-((dimethylamino)methylene)-6,11-dihydro-5H-dipyrido[2,3-b:4′,3′-f]azepin-5-one (0.745 g) as a brown solid, which was used without further purification in Step 2.
WORKUP
后处理
- temperatureThe reaction mixture was cooled
- customsolvent removed under reduced pressure