反应详情

温度

80 °C

To a solution of o-phenylenediamine (4 g, 37.03 mmol) in DMF (30 mL) was added triethylamine (10.3 mL, 74.06) followed by ethyl-2-bromo acetate (4.53 mL, 40.73 mmol). The reaction was stirred at RT for 16 h and at 80° C. for 3 h. The reaction was monitored by TLC. After completion of reaction, the DMF was removed under vacuum. Water (20 mL) was added to the reaction mixture, which was then extracted with EtOAc (300 mL). The organic layer was dried over sodium sulfate, concentrated under vacuum, and the product recrystallized with DCM/hexane in 1:1 ratio to obtain 2.2 g of desired compound.

1. customAfter completion of reaction
2. customthe DMF was removed under vacuum
3. additionWater (20 mL) was added to the reaction mixture, which
4. extractionwas then extracted with EtOAc (300 mL)
5. dry with materialThe organic layer was dried over sodium sulfate
6. concentrationconcentrated under vacuum
7. customthe product recrystallized with DCM/hexane in 1:1 ratio