反应详情

To a suspension of (E)-N,N-Dimethyl-N′-(4-methyl-5-nitro-6-oxo-1,6-dihydropyrimidin-2-yl)formimidamide (53.4 g, 0.24 mmol) in DMF (690 mL) was added DBU (44.6 mL, 0.30 mol) and benzyl bromide (44.4 mL, 0.29 mol) and stirred at room temperature for 1 h. The excess of DBU was neutralized with HCl, and the mixture was concentrated in vacuo. The residue was dissolved in methylene chloride and extracted twice with 2M HCl and water, then dried over Na2SO4 and concentrated. Trituration with ethanol afforded the crystalline product which was washed with ethanol to give the product (64.7 g, 86% yield) and used in the next step without further purification.

1. concentrationthe mixture was concentrated in vacuo
2. dissolutionThe residue was dissolved in methylene chloride
3. extractionextracted twice with 2M HCl and water
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customTrituration with ethanol afforded the crystalline product which
7. washwas washed with ethanol