反应详情

温度

50 °C

0.26 g of sodium hydride (50% suspension in oil) is added to a solution of 0.75 g of 6-hydroxy-1,2,3,4-tetrahydroisoquinoline in 30 ml of dimethylformamide, and the mixture is stirred at 50° C. for 30 minutes. Then 2.04 g of (2RS,4SR)-2-(2,4-dichlorophenyl)-2-(1H-imidazol-1-ylmethyl)-1,3-dioxolan-4-ylmethyl methanesulfonate are introduced, and the mixture is stirred at 80° C. for 5 hours. It is allowed to cool, 1.00 g of finely powdered potassium carbonate and 1.00 g of 4-chloromethylbiphenyl are added, and the mixture is stirred at 60° C. for a further 5 hours. After cooling, the solvent is removed at the oil pump in a rotary evaporator, and the residue is taken up with a mixture of 50 ml of water and 50 ml of methylene chloride. The organic phase is washed twice more with water, dried over magnesium sulfate and evaporated in a rotary evaporator. To purify the crude product, it is chromatographed on silica gel using a mixture of ethyl acetate and methanol 19:1. 1.7 g of a viscous oil (57% of theory) which gradually crystallizes is obtained. Melting point 103°-105°.

1. stirringthe mixture is stirred at 80° C. for 5 hours
2. temperatureto cool
3. stirringthe mixture is stirred at 60° C. for a further 5 hours
4. temperatureAfter cooling
5. customthe solvent is removed at the oil pump in a rotary evaporator
6. additionthe residue is taken up with a mixture of 50 ml of water and 50 ml of methylene chloride
7. washThe organic phase is washed twice more with water
8. dry with materialdried over magnesium sulfate
9. customevaporated in a rotary evaporator
10. customTo purify the crude product, it
11. customis chromatographed on silica gel using
12. additiona mixture of ethyl acetate and methanol 19:1
13. custom1.7 g of a viscous oil (57% of theory) which gradually crystallizes
14. customis obtained