Methanol → HCID 178441203, compound

First, 7.2 g of formamidine hydrochloride, 7.5 g of sodium methoxide, and 70 mL of methanol were put into a 100 mL three-neck flask. Then, 10 g of methyl 4,4-dimethyl-3-oxovalerate was added to this mixed solution. The mixture was stirred at room temperature for 24 hours. After that, a mixed solution of 17 mL of water and 7.2 mL of acetic acid was added to the reacted solution, and the mixture was stirred at room temperature. This mixture was concentrated, and the resulting residue was dissolved in water. The solution was subjected to extraction with ethyl acetate. The obtained solution of the extract was washed with saturated brine, and magnesium sulfate was added for drying. After the drying, the solution was filtered. After the solvent of this solution was distilled off, the obtained solid was washed with ethyl acetate, so that the pyrimidine derivative to be produced was obtained as a white solid in a yield of 49%. A synthesis scheme of Step 1 is shown in (k-1).

1. stirringthe mixture was stirred at room temperature
2. concentrationThis mixture was concentrated
3. dissolutionthe resulting residue was dissolved in water
4. extractionThe solution was subjected to extraction with ethyl acetate
5. washThe obtained solution of the extract was washed with saturated brine, and magnesium sulfate
6. additionwas added
7. customfor drying
8. filtrationAfter the drying, the solution was filtered
9. distillationAfter the solvent of this solution was distilled off
10. washthe obtained solid was washed with ethyl acetate, so that the pyrimidine derivative
11. customto be produced
12. customwas obtained as a white solid in a yield of 49%
13. customA synthesis scheme of Step 1

ORD record

ord-71d4a0ad68624f4e834f4e7ea6710890

Source dataset

uspto-grants-2015_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09127032B2