反应详情

温度

80 °C

0.55 g of sodium hydride (50% suspension in oil) is added to a solution of 1.50 g of 6-hydroxy-1,2,3,4-tetrahydroisoquinoline in 30 ml of dimethyl sulfoxide, and the mixture is stirred at 50° C. until evolution of hydrogen has finished. 4.07 g of (2RS,4SR)-2-(2,4-dichlorophenyl)-2-(1H-imidazol-1-ylmethyl)-1,3-dioxolan-4-ylmethyl methanesulfonate are added and the mixture is stirred at 80° C. for 5 hours. The solvent is removed under oil pump vacuum, the residue is taken up with a mixture of 50 ml of water and 50 ml of methylene chloride, and the organic phase is extracted twice more by shaking with water, dried and evaporated in a rotary evaporator. The residue is chromatographed on silica gel using methanol as the mobile phase. 2.45 g of colorless oil (53% of theory), which gradually crystallizes, are obtained. Melting point 143°-145° C.

1. customThe solvent is removed under oil pump vacuum
2. additionthe residue is taken up with a mixture of 50 ml of water and 50 ml of methylene chloride
3. extractionthe organic phase is extracted twice more
4. stirringby shaking with water
5. customdried
6. customevaporated in a rotary evaporator
7. customThe residue is chromatographed on silica gel
8. custom2.45 g of colorless oil (53% of theory), which gradually crystallizes
9. customare obtained