反应详情

0.35 g (8.0 mmol) sodium hydride (55%, suspension in mineral oil) were added to 2.2 g (7.6 mmol) of 6-(6-chloropyrimidine-4-carbonyl)-4-methyl-3H-benzoxazol-2-one in 10 mL N,N′-dimethylformamide. The reaction mixture was stirred for 30 min at RT. Then 0.95 mL (15.0 mmol) iodomethane were added and the mixture was stirred for 1 h at RT. The reaction mixture was combined with ice water, the aqueous phase was extracted several times with EtOAc. The combined organic phases were dried on sodium sulphate, filtered and concentrated to dryness by rotary evaporation. The residue was triturated with diethyl ether, suction filtered and dried.

1. stirringthe mixture was stirred for 1 h at RT
2. extractionthe aqueous phase was extracted several times with EtOAc
3. customThe combined organic phases were dried on sodium sulphate
4. filtrationfiltered
5. concentrationconcentrated to dryness by rotary evaporation
6. customThe residue was triturated with diethyl ether, suction
7. filtrationfiltered
8. customdried