Water → HCID 19955490, compound

A stirred solution of 0.50 gram (0.003 mole) of 2,4-diamino-5-hydroxypyrimidine hydrosulfate salt, 0.47 gram (0.007 mole) of 1-bromo-2-ethylbutane and 0.95 gram (0.007 mole) of anhydrous potassium carbonate in 5 mL of N,N-dimethylformamide was heated at 84°-86° C. for about two hours. After this time the reaction mixture was allowed to cool to ambient temperature as it stirred during about a 16 hour period. The reaction mixture was then stirred with 50 mL of water and 50 mL of methylene chloride. The methylene chloride layer was separated and washed with 50 mL of water. The organic layer was dried with sodium sulfate and filtered. The filtrate was concentrated under reduced pressure to a solid residue. The residue was recrystallized from 2:1 water and methanol, yielding, when dried, 0.20 gram of 2,4-diamino-5-(2-ethylbutoxy)pyrimidine. The NMR spectrum was consistent with the proposed structure.

1. customThe methylene chloride layer was separated
2. washwashed with 50 mL of water
3. dry with materialThe organic layer was dried with sodium sulfate
4. filtrationfiltered
5. concentrationThe filtrate was concentrated under reduced pressure to a solid residue
6. customThe residue was recrystallized from 2:1 water and methanol
7. customyielding
8. customwhen dried

ORD record

ord-5c5e8f4fd58e4eb182aa223144c7b05b

Source dataset

uspto-grants-1996_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05521192