反应详情

0.004 mole of (1R,5S)-3-azabicyclo[3.1.0]hexane and 0.002 mole of sodium iodide are added to the reaction mixture of Step 1 at ambient temperature. Refluxing is then resumed for 16 hours. The precipitate is filtered off and rinsed with acetonitrile. The filtrate is concentrated to dryness. The residue is taken up in dichloromethane. The resulting solution is extracted with sodium hydroxide solution and then with water, before being dried over magnesium sulphate and concentrated to dryness. The residue is purified by a preparative chromatography technique on a Lichroprep RP-18 phase.

1. temperatureRefluxing
2. filtrationThe precipitate is filtered off
3. washrinsed with acetonitrile
4. concentrationThe filtrate is concentrated to dryness
5. extractionThe resulting solution is extracted with sodium hydroxide solution
6. dry with materialwith water, before being dried over magnesium sulphate
7. concentrationconcentrated to dryness
8. customThe residue is purified by a preparative chromatography technique on a Lichroprep RP-18 phase