反应详情

1.89 g of 2-allyl-6-hydroxy-1,2,3,4-tetrahydroisoquinoline are added to a freshly prepared solution of alcoholate from 0.23 g of sodium in 30 ml of dry ethanol, the mixture is stirred for 15 minutes, 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 then heated under reflux for 8 hours. After cooling, the ethanol is removed 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 shaken twice more with water, dried over magnesium sulfate and evaporated in a rotary evaporator. The residue is purified by column chromatography on silica gel using a mixture of ethyl acetate/methanol 4:1. 1.3 g of a colorless resin (26% of theory) which gradually crystallizes is obtained. Melting point 94°-95° C.

1. temperaturethe mixture is then heated
2. temperatureunder reflux for 8 hours
3. temperatureAfter cooling
4. customthe ethanol is removed in a rotary evaporator
5. additionthe residue is taken up with a mixture of 50 ml of water and 50 ml of methylene chloride
6. stirringThe organic phase is shaken twice more with water
7. dry with materialdried over magnesium sulfate
8. customevaporated in a rotary evaporator
9. customThe residue is purified by column chromatography on silica gel using
10. additiona mixture of ethyl acetate/methanol 4:1
11. custom1.3 g of a colorless resin (26% of theory) which gradually crystallizes
12. customis obtained