反应详情

温度

66 °C

To a 2-L reactor with a stirrer, a thermocouple, a condenser and nitrogen inlet were charged 8-bromo-5fluoroquinoline (50 g), tetrahydrofuran (795 g), Pd2(dba)3 (3.78 g), Cymap (1.6 g), and 1,4-Dioxa-8-azaspiro[4.5]decane (47.3 g). the mixture was heated to reflux (66° C.) and the reaction was complete. The reaction mixture was quenched into a 5 L reactor containing 1000 g of water and 640 g of MTBE. The bottom aqueous layer was split off and the organic layer was washed with 5% NaOH (1120 g) and 20% NaCl (2×100 g). The solvent was evaporated, weight 87 g vs 79.4 g by theory.

1. temperaturethe mixture was heated
2. customThe reaction mixture was quenched into a 5 L reactor
3. additioncontaining 1000 g of water and 640 g of MTBE
4. customThe bottom aqueous layer was split off
5. washthe organic layer was washed with 5% NaOH (1120 g) and 20% NaCl (2×100 g)
6. customThe solvent was evaporated