反应详情

10.0 g (47.5 mmol) 2,6-dichloropyridine-4-carboxylic acid chloride, 7.08 g (47.5 mmol) 4-methyl-3H-benzoxazol-2-one and 32.0 g (240 mmol) aluminium trichloride were heated to 120° C. for 1 h with stirring. The mixture was mixed with ice water and extracted several times with EtOAc. The solid precipitated from EtOAc was suction filtered and washed with EtOAc. The organic phase remaining was separated off, dried on sodium sulphate, filtered and evaporated down. The residue was combined with a little EtOAc, the precipitated solid was suction filtered and washed with a little EtOAc. For further purification the mixture was recrystallised from EtOAc.

1. extractionextracted several times with EtOAc
2. customThe solid precipitated from EtOAc
3. filtrationfiltered
4. washwashed with EtOAc
5. customThe organic phase remaining was separated off
6. customdried on sodium sulphate
7. filtrationfiltered
8. customevaporated down
9. filtrationfiltered
10. washwashed with a little EtOAc
11. customFor further purification the mixture
12. customwas recrystallised from EtOAc