Sodium Hydroxide → HCID 59326879, compound

2,4-Dimethoxy-5-iodopyrimidine Z (2.54 g, 9.6 mmol) was added to 26 ml of 5N sodium hydroxide in 50% aqueous methanol and the resulting solution was refluxed overnight. The reaction mixture was evaporated to dryness under reduced pressure, diluted to 25 ml with water and neutralized to ph ˜6 with 1N hydrochloric acid. The precipitate was filtered off, washed with water (2×10 ml), methanol (2×10 ml) and diethyl ether to give 0.55 g of pure product. The filtrate was concentrated under reduced pressure and kept overnight at 4° C. The crystals of the product were filtered off washed as above to give additional 0.3 g of pure product as a colorless crystals (total yield 0.85 g, 35%). 1HNMR (DMSO-d6, 300 MHz) δ 8.14 (s, 1H) 3.82 (s, 3H); 3.3 (broad s, 1H).

1. temperaturethe resulting solution was refluxed overnight
2. customThe reaction mixture was evaporated to dryness under reduced pressure
3. additiondiluted to 25 ml with water and neutralized to ph ˜6 with 1N hydrochloric acid
4. filtrationThe precipitate was filtered off
5. washwashed with water (2×10 ml), methanol (2×10 ml) and diethyl ether

ORD record

ord-c7e6dcdc53594075bea28e5f80c7ff70

Source dataset

uspto-grants-2013_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08466163B2