反应详情

温度

55 °C

A solution of 2-hydroxypyrimidine (0.16 mol) in methanol (300 ml) was stirred at room temperature for 30 minutes. A solution of Na2CO3 (0.16 mol) in methanol (40 ml) was added. The mixture was stirred and refluxed for 15 minutes and cooled to 55° C. A solution of N,N-bis(phenylmethyl)-2-oxiranemethanamine (0.16 mol) in toluene (320 ml) was added dropwise. The mixture was stirred at 50° C. overnight Water (150 ml) was added The mixture was stirred at 55° C. for 15 minutes. The organic layer was separated, washed with water, dried, filtered and the solvent was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 97/3). The pure fractions were collected and the solvent was evaporated, yielding 26.55 g of (±)-[3-[bis(phenylmethyl)amino]-2-hydroxypropyl]-2(1H)pyrimidinone (intermediate 4).

1. temperaturerefluxed for 15 minutes
2. additionwas added The mixture
3. stirringwas stirred at 55° C. for 15 minutes
4. customThe organic layer was separated
5. washwashed with water
6. customdried
7. filtrationfiltered
8. customthe solvent was evaporated
9. customThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 97/3)
10. customThe pure fractions were collected
11. customthe solvent was evaporated