反应详情

Add 1-hydroxypropan-2-one (24.3 mL, 355 mmol) and 4-amino-2-(methylthio)pyrimidine-5-carbaldehyde (50 g, 296 mmol) to a solution of sodium hydroxide (23.64 g, 591 mmol) and water (200 mL). Add EtOH (600 mL) to the suspension and stir at RT overnight. Slowly add a solution of concentrated HCl (50 mL) in water (350 mL). Add 1:1 EtOH/H2O (100 mL) and collect the solids by filtration. Wash the solids with 1:1 EtOH/H2O (250 mL), ice cold EtOH (4×25 mL) and hexanes (2×250 mL). Dry in the vacuum oven at 30-35° C. to provide the title compound as a tan solid (34 g, 56% yield). MS (m/z): 208.1 (M+1).

1. customcollect the solids
2. filtrationby filtration
3. washWash the solids with 1:1 EtOH/H2O (250 mL), ice cold EtOH (4×25 mL) and hexanes (2×250 mL)
4. customDry in the vacuum oven at 30-35° C.