5-Chloro-2(1H)-pyrimidinone → HCID 20491782, 화합물

A suspension of 5-chloropyrimidin-2-one (1.007 g) and sodium hydrogen carbonate (647 mg) in 3-methylene-γ-butyrolactone (1.208 g) and ethanol (50 ml) was stirred and heated at reflux. After 2 h, the suspension was cooled and filtered. The filtrate was evaporated and the residue and solid were combined and boiled in ethyl acetate (150 ml). The resulting suspension was filtered and the filtrate evaporated to a pale cream solid. The solid from the filtration was treated with water (50 ml) and the resulting suspension filtered to give a solid which was combined with the pale cream solid and recrystallised from methanol to give white crystals of the title pyrimidinone (424 mg), m.p. 283°-284° C., λmax (EtOH) 229.5 nm (ε 7,700), 332 nm (ε 2,100).

1. temperatureheated
2. temperatureat reflux
3. temperaturethe suspension was cooled
4. filtrationfiltered
5. customThe filtrate was evaporated
6. filtrationThe resulting suspension was filtered
7. customthe filtrate evaporated to a pale cream solid
8. filtrationThe solid from the filtration
9. additionwas treated with water (50 ml)
10. filtrationthe resulting suspension filtered
11. customto give a solid which
12. customrecrystallised from methanol

ORD 기록

ord-e97544ef8469477ca75b12a99d36b46d

출처 데이터셋

uspto-grants-1983_08

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US04399140