Hydrochloric Acid → 4-Pyrimidinemethanol, 2-amino-

2-Amino-4-methoxycarbonylpyrimidine (3.0 g, 20 mmol, Reference Compound No. 3-1) was suspended in a mixture solvent of ethanol (150 mL) and dichloromethane (20 mL), then sodium borohydride (2.2 g, 59 mmol) was added thereto at room temperature, and the whole was stirred for 24 hours. Acetone (20 mL) was added gradually under ice-cooling, and then 2M hydrochloric acid was added until the bubbles were no longer formed. Saturated aqueous sodium hydrogencarbonate solution was added to adjust the pH of the reaction mixture to 8, and the precipitated solid was filtered out. The filtrate was concentrated under reduced pressure, then suspended in a 10% methanol-chloroform solution, and the mixture was filtered again with silica gel (5.0 g). The filtrate was evaporated under reduced pressure, the precipitated solid was filtered off with ethyl acetate, and dried under reduced pressure to give 1.8 g of the title Reference Compound as a pale yellow solid (Yield: 73%)

1. temperaturecooling
2. customwere no longer formed
3. filtrationthe precipitated solid was filtered out
4. concentrationThe filtrate was concentrated under reduced pressure
5. filtrationthe mixture was filtered again with silica gel (5.0 g)
6. customThe filtrate was evaporated under reduced pressure
7. filtrationthe precipitated solid was filtered off with ethyl acetate
8. customdried under reduced pressure

ORD-Eintrag

ord-1eff8aa604f84a80b31f972bf47ab66b

Quelldatensatz

uspto-grants-2011_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07906511B2