反应详情

0.175 g (4.00 mmol) sodium hydride (55%, suspension in mineral oil) were added at RT to 1.33 g (3.80 mmol) 6-(3-bromo-4-fluoro-benzoyl)-4-methyl-3H-benzoxazol-2-one in 5 mL DMF. The reaction mixture was stirred for 30 min at RT. Then 0.317 mL (5.00 mmol) iodomethane were added and the mixture was stirred for 1 h at RT. Then 0.100 mL (15.8 mmol) iodomethane were added and the mixture was stirred overnight at RT. After the addition of ice water the reaction mixture was extracted with EtOAc. The organic phase was washed with water, dried on sodium sulphate and evaporated down i. vac. The residue was purified by flash chromatography. The fractions containing the product were combined, evaporated down and dried i. vac.

1. stirringthe mixture was stirred for 1 h at RT
2. stirringthe mixture was stirred overnight at RT
3. extractionwas extracted with EtOAc
4. washThe organic phase was washed with water
5. customdried on sodium sulphate
6. customevaporated down i
7. customThe residue was purified by flash chromatography
8. additionThe fractions containing the product
9. customevaporated down
10. customdried i