反应详情

0.131 g (3.00 mmol) sodium hydride (55%, suspension in mineral oil) were added to 0.677 g (2.00 mmol) 4,6-diiodopyrimidine, 0.535 g (3.00 mmol) 8-methyl-2,3-dihydro-benzo[1,4]dioxin-6-carbaldehyde (US2005/256099) and 0.133 g (1.00 mmol) 1,3-dimethylimidazolium chloride in 10 mL THF and the mixture was refluxed for 4 h. Then the reaction mixture was mixed with ice water and extracted with EtOAc. The organic phase was dried on sodium sulphate, evaporated down i. vac. and the residue was purified by preparative HPLC-MS. The fractions containing the product were combined and the organic solvent was evaporated down i. vac. The residue was made alkaline with 1N aqueous sodium hydroxide solution and the grease precipitated was extracted with EtOAc. The organic phase was dried on sodium sulphate, filtered, evaporated down and dried i. vac.

1. temperaturethe mixture was refluxed for 4 h
2. extractionextracted with EtOAc
3. customThe organic phase was dried on sodium sulphate
4. customevaporated down i
5. customand the residue was purified by preparative HPLC-MS
6. additionThe fractions containing the product
7. customthe organic solvent was evaporated down i
8. customthe grease precipitated
9. extractionwas extracted with EtOAc
10. customThe organic phase was dried on sodium sulphate
11. filtrationfiltered
12. customevaporated down
13. customdried i