反应详情

温度

95 °C

To a mixture of 2-(4,4-dimethylcyclohexyl)-5-methyl[1,3]thiazolo[5,4-d]pyrimidin-7-ol (16.2 g) and toluene (160 mL) were added DMF (10 mL) and phosphorous oxychloride (11 mL), followed by stirring at 95° C. for 30 minutes. The reaction mixture was concentrated under reduced pressure. To the residue was added chloroform, and the mixture was neutralized with a 1 M aqueous NaOH solution in an ice bath and extracted with chloroform. The organic layer was dried over MgSO4 and then concentrated under reduced pressure. The residue was purified by silica gel column (hexane/EtOAc) to obtain 7-chloro-2-(4,4-dimethylcyclohexyl)-5-methyl[1,3]thiazolo[5,4-d]pyrimidine (13.2 g).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additionTo the residue was added chloroform
3. customthe mixture was neutralized with a 1 M aqueous NaOH solution in an ice bath
4. extractionextracted with chloroform
5. dry with materialThe organic layer was dried over MgSO4
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by silica gel column (hexane/EtOAc)