反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
{(R)-2-[5-(4-chloro-butyrylamino)-3-(2,6-difluoro-benzyl)-2,6-dioxo-3,6-dihydro-2H-pyrimidin-1-yl]-1-phenyl-ethyl}-carbamic acid tert-butyl ester (30 mg, 0.052 mmol) and potassium carbonate (30 mg, 0.217 mmol) were dissolved at room temperature for 6 hrs in DMF (1 mL) with stirring. The solution was diluted with dichloromethane and washed with water to separate an organic layer. After concentration of the organic layer, the residue was purified using silica gel chromatography (eluent: dichloromethane/methanol, 30/1) and dried in a vacuum to afford 25 mg of the compound as a colorless oil (yield 90%). 1H NMR (300 MHz, CDCl3) δ 1.34 (9H, s), 2.15 (2H, p), 2.51 (2H, t), 3.80 (2H, m), 4.03 (1H, m), 4.27 (1H, m), 4.98-5.13 (3H, m), 5.57 (1H, d), 6.97 (2H, m), 7.22-7.40 (6H, m), 7.62 (1H, s)
WORKUP
后处理
- washwashed with water
- customto separate an organic layer
- customAfter concentration of the organic layer, the residue was purified
- customdried in a vacuum