反应详情

With reference to Scheme 3, to a solution of 2800 g (21.13 mol) of 2-hydroxypyrimidine hydrochloride in 8400 mL of concentrated sulfuric acid was added dropwise 3434 g (52.83 mol) of fuming nitric acid. The solution was heated at reflux for 16 h, then it was allowed to cool to room temperature and was poured slowly into cold water (30 L). The mixture was basified with 50% NaOH to pH 2.5. Isopropyl alcohol (16 L) was added and the mixture was stirred for 60 minutes after which the layers were allowed to separate. The organic layer was diluted with ethyl acetate (16 L) and washed with brine. The organics were concentrated under reduced pressure to yield 2689 g of crude product, which was used in the next step without purification.

1. temperatureThe solution was heated
2. temperatureat reflux for 16 h
3. customto separate
4. additionThe organic layer was diluted with ethyl acetate (16 L)
5. washwashed with brine
6. concentrationThe organics were concentrated under reduced pressure