Hydrochloric Acid → 2-(Propylthio)pyrimidine-4,6-diol

Water (670 ml) was added to 2-thiobarbituric acid (200 g). The resulting mixture was stirred and sodium hydroxide (126.3 g) was added in portions. The mixture was stirred for 40 min. then diluted with water. 1-Methyl-2-pyrrolidinone (400 ml) and 1-iodopropane (140.9 ml) were then added. The resulting slurry was stirred at 20° C. for 22 h. The pH of the mixture was then adjusted to 6.5 by addition of 1M HCl (600 ml) over 30 min, then to pH 2.5 by the addition of 6 M HCl (180 ml) over a further 30 min. The resulting slurry was stirred for 18 h and the product was isolated by filtration and washed successively with water (4×100 ml), ethanol (200 mm) and water (2×200 ml). The product was dried under reduced pressure overnight at 50° C. to yield the title product as a white powder (185 g).

1. stirringThe mixture was stirred for 40 min.
2. stirringThe resulting slurry was stirred at 20° C. for 22 h
3. stirringThe resulting slurry was stirred for 18 h
4. customthe product was isolated by filtration
5. washwashed successively with water (4×100 ml), ethanol (200 mm) and water (2×200 ml)
6. customThe product was dried under reduced pressure overnight at 50° C.

ORDレコード

ord-f00ef7c9f6644b0ca06ea85b078d0d7b

出典データセット

uspto-grants-2008_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07381828B2