反应详情

温度

40 °C

Triethylamine (1 mmol) was added to a mixture of 5-trifluoromethyl pyrimidin-2-one (see Preparation 11 of European Patent Publication Ser. No. 0 056 319) (1 mmol) in dichloromethane (10 ml) and the solution stirred for 5 minutes before 4-chlorobenzyl chloromethyl ether (see Preparation 5a and 5b) (1 mmol) in dichloromethane (2 ml) was added. The mixture was stirred at room temperature overnight and at 40° C. for 3 hours before the solvent was distilled off and the residue triturated with water. The product was extracted into chloroform, dried (MgSO4) and evaporated. The residue was washed with ether and dried; yield 91%, m.p. 120° C. 1H NMR (CDCl3): δ4.64 (CH2Ph), 5.38 (NCH2), 7.24 (Ph), 8.11 (H-4, J 3 Hz), 8.74 (H-6, J 3 Hz). IR (KBr): 1680 cm-1 (CO).

1. customPreparation 11 of European Patent Publication Ser
2. additionwas added
3. distillationwas distilled off
4. customthe residue triturated with water
5. extractionThe product was extracted into chloroform
6. dry with materialdried (MgSO4)
7. customevaporated
8. washThe residue was washed with ether
9. customdried