HRID1175629
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
PROCEDURE
实验过程
5-(5-Bromopyridin-2(1H)-ylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (example 42f) (3.55 g, 11.87 mmol) was suspended in conc. HCl (55 mL) and refluxed for 3 h. The solution was concentrated under reduced pressure and a residue was triturated with EtOH to provide white crystals that were filtered off and washed with EtOH (2.34 g, 78%). 1H NMR (400 MHz, dMSO): δ 3.81 (s, 2H), 7.44-7.46 (d, 1H), 8.12-8.15 (dd, 1H), 8.70-8.71 (d, 1H), 11.30 (bs, 1H); MS+H (218).
WORKUP
后处理
- temperaturerefluxed for 3 h
- concentrationThe solution was concentrated under reduced pressure
- customa residue was triturated with EtOH
- customto provide white crystals that
- filtrationwere filtered off
- washwashed with EtOH (2.34 g, 78%)