Methanol → HCID 178441203, Verbindung

First, 7.2 g of formamidine acetate, 7.5 g of sodium methoxide, and 70 mL of methanol were put in a 100 mL three-neck flask. Then, 10 g of methyl 4,4-dimethyloxovalerate was added to this mixed solution. The mixture was stirred at room temperature for 24 hours. After a predetermined time elapsed, a mixed solution of 17 mL of water and 7.2 mL of acetic acid was added to the mixture, and the mixture was stirred at room temperature. This mixture was condensed, and the given 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 anhydrate magnesium sulfate was added to the organic layer for drying. The obtained mixture was subjected to gravity filtration, and the filtrate was condensed to give a solid. This solid was washed with ethyl acetate to give 4-hydroxy-6-tert-butylpyrimidine (white solid, yield of 49%). A synthetic scheme of Step 1 is shown in (a-1) below.

1. stirringthe mixture was stirred at room temperature
2. customcondensed
3. extractionThe solution was subjected to extraction with ethyl acetate
4. washThe obtained solution of the extract was washed with saturated brine, and anhydrate magnesium sulfate
5. additionwas added to the organic layer
6. customfor drying
7. filtrationThe obtained mixture was subjected to gravity filtration
8. customcondensed
9. customto give a solid
10. washThis solid was washed with ethyl acetate

ORD-Eintrag

ord-36ad53daad64456a959435a30ca8b90b

Quelldatensatz

uspto-grants-2014_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08889858B2