反应详情

Sodium metal (1.6 g, 0.068 mol) was added to 4 Å molecular sieves (12 g) and ethanol (200 mL) under nitrogen. The mixture was stirred for 15 minutes, then hydroxyguanidine sulfate (9.32 g, 0.035 mol) added and the mixture stirred for 30 minutes. Methyltetradecanoate (1.43 g, 0.006 mol) was then added and the mixture refluxed for 1.5 hours, allowed to cool, filtered, and concentrated. The concentrate was partitioned between CH2Cl2 and water. The organic layer was washed with water and brine, dried with Na2SO4, filtered, concentrated, and triturated with hexane. The resulting solid was filtered, washed with hexane, and dried in vacuo to yield 0.23 g, m.p. 90°-91° C.

1. stirringthe mixture stirred for 30 minutes
2. temperaturethe mixture refluxed for 1.5 hours
3. temperatureto cool
4. filtrationfiltered
5. concentrationconcentrated
6. customThe concentrate was partitioned between CH2Cl2 and water
7. washThe organic layer was washed with water and brine
8. dry with materialdried with Na2SO4
9. filtrationfiltered
10. concentrationconcentrated
11. customtriturated with hexane
12. filtrationThe resulting solid was filtered
13. washwashed with hexane
14. customdried in vacuo
15. customto yield 0.23 g, m.p. 90°-91° C.