反应详情

温度

70 °C

A 1 L flask equipped with a mechanical stirrer and a thermometer was charged with 2,4-dibromothiazole (60 g, 0.247 mol) and DMF (480 mL). After dissolution, cis-2,6-dimethylmorpholine (33.65 mL, 0.272 mol) and DIPEA (61.23 mL, 0.37 mol) were added under a stream of nitrogen. The reaction mixture was heated to 70° C. under nitrogen and stirred overnight. The reaction mixture was cooled to 10° C. in an ice/water bath. Then water (1 L) was added dropwise in a temperature range of 10-20° C. A slightly exothermic reaction was observed, with formation of an off-white precipitate. After the addition, the reaction mixture was stirred for 30 min. The precipitate was then filtered and washed with water (50 ml). The collected solid was dried in a vacuum oven at 50° C., yielding 52.8 g (77%) of Intermediate 1 as an off-white solid.

1. customA 1 L flask equipped with a mechanical stirrer
2. additionwere added under a stream of nitrogen
3. temperatureThe reaction mixture was cooled to 10° C. in an ice/water bath
4. customA slightly exothermic reaction
5. additionAfter the addition
6. stirringthe reaction mixture was stirred for 30 min
7. filtrationThe precipitate was then filtered
8. washwashed with water (50 ml)
9. customThe collected solid was dried in a vacuum oven at 50° C.