反应详情

To a solution of 3-benzyloxycarbonylamino-6-methyl-1-(tert-butoxycarbonylmethyl)-2-pyridinone (6.0 g, 17 mmol), as prepared in step 2 of Example 1, in methylene chloride (12 mL) was added trifluoroacetic acid (12 mL) and the reaction stirred at ambient temperature. After 30 minutes the reaction was concentrated in vacuo, dissolved in methylene chloride, and diluted with hexane. The precipitated product was collected by filtration and dried in vacuo giving a quantitative yield of white solid. 1H NMR (300 MHz, DMSO-d6) δ13.17 (br s, 1 H), 8.36 (s, 1H), 7.74 (d, 1H, J=7.5 Hz), 7.35 (m, 5H), 6.18 (d, 1H, J=7.7Hz), 5.15 (s, 2H), 4.77 (s, 2H), 2.25 (s, 3H).

1. concentrationAfter 30 minutes the reaction was concentrated in vacuo
2. dissolutiondissolved in methylene chloride
3. additiondiluted with hexane
4. filtrationThe precipitated product was collected by filtration
5. customdried in vacuo