Methanol → HCID 178441203、化合物

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 the 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 a saturated aqueous solution of sodium chloride, and anhydrous magnesium sulfate was added to the organic layer for drying. The obtained mixture was subjected to gravity filtration, and the filtrate was concentrated to give a solid. This solid was washed with ethyl acetate to give 4-tert-butyl-6-hydroxypyrimidine (white powder, yield of 49%). Synthesis Scheme (a-1) of Step 1 is shown 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 a saturated aqueous solution of sodium chloride, and anhydrous magnesium sulfate
5. additionwas added to the organic layer
6. customfor drying
7. filtrationThe obtained mixture was subjected to gravity filtration
8. concentrationthe filtrate was concentrated
9. customto give a solid
10. washThis solid was washed with ethyl acetate

ORDレコード

ord-6e6da08b7f2f4918ac1c34aed9140b28

出典データセット

uspto-grants-2015_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09130182B2