反应详情

温度

0 °C

Into a 1.0 L round bottom flask equipped with mechanical stirrer, addition funnel, thermometer and nitrogen inlet tube was placed 100 grams (0.67 Mol) of 5-amino-2-methylbenzoxazole and 350 mL of pyridine. The slurry was stirred in an ice/ethanol bath at 0° C. then 110 grams (0.69 Mol) of Intermediate 1 was added dropwise so as to maintain a reaction temperature below 7° C. The reaction was stirred at 0° C. for two hours then the resulting red colored mixture was poured into 1.0 L of ethyl acetate. The slurry was stirred for 30 minutes then filtered and the collected solids were discarded. The filtrate was extracted with 4×200 mL of 10% hydrochloric acid and the organic phase was collected and dried over magnesium sulfate. The solvents were removed in vacuo to afford 140 grams (0.52 Mol, 76.7% yield) of desired product as a tan solid.

1. customInto a 1.0 L round bottom flask equipped with mechanical stirrer, addition funnel
2. customthermometer and nitrogen inlet tube was placed
3. temperatureto maintain a reaction temperature below 7° C
4. stirringThe reaction was stirred at 0° C. for two hours
5. stirringThe slurry was stirred for 30 minutes
6. filtrationthen filtered
7. extractionThe filtrate was extracted with 4×200 mL of 10% hydrochloric acid
8. customthe organic phase was collected
9. dry with materialdried over magnesium sulfate
10. customThe solvents were removed in vacuo