反应详情

温度

157.5 °C

Ethyl 2-(1-(2-chloroethoxy)-2-methylpropan-2-yl)-5-hydroxy-6-oxo-1,6-dihydropyrimidine-4-carboxylate Diethyl 2-(3-(2-chloroethoxy)-2,2-dimethylpropanimidamidooxy)but-2-enedioate was dissolved in 150 mL 1,2,4-trimethylbenzene and heated at 155-160° C. for 2.5 hrs with stirring under N2. The solvent was evaporated at reduced pressure and the residue was dissolved in EtOAc and extracted 2× with dil NaHCO3. The aqueous extracts were acidified with HCl and extracted with CH2Cl2. After drying (MgSO4), filtration and concentration provided the title compound (1.9 g, 43%) as a white solid. 1H NMR (300 MHz, CDCl3) δ: 1.31 (s, 6H), 1.41 (t, J=7.1 Hz, 3H), 3.54 (s, 2H), 3.63-3.72 (m, 2H), 3.75-3.83 (m, 2H), 4.42 (q, J=7.3 Hz, 2H). LC/MS (M+H): 319.

1. customThe solvent was evaporated at reduced pressure
2. dissolutionthe residue was dissolved in EtOAc
3. extractionextracted 2× with dil NaHCO3
4. extractionextracted with CH2Cl2
5. customAfter drying
6. filtration(MgSO4), filtration and concentration