反应详情

Into 150 mL of DMF, 65 g (515 mmol) of 2-furoic hydrazide and 70 mL (510 mmol) of DBU were dissolved, and a DMF solution of 4,6-dichloro-2-methylthiopyrimidine (50.0 g (256 mmol)/100 mL) was slowly added dropwise thereto at room temperature (inner temperature was controlled at 45° C. or lower). After stirring at room temperature for about 2 hours, the reaction solution was poured into ice-water and the pH was adjusted to 6 to 7 with a 2 mol/L hydrochloric acid solution, followed by collecting the resulting solid through filtration. The collected solid was dissolved into an organic solvent (chloroform/methanol=10/1) and, after washing with water, the solution was dried over anhydrous magnesium sulfate. The solvent was evaporated, and the resulting residue was triturated twice with chloroform to obtain 56.9 g of Compound A as white flocculent crystals (yield: 78%). The residue obtained by concentrating the filtrate was purified by silica gel column chromatography (hexane/ethyl acetate=6/4) to additionally recover Compound A in about 10% yield.

1. customat room temperature
2. custom(inner temperature was controlled at 45° C. or lower)
3. customby collecting the resulting solid
4. filtrationthrough filtration
5. dissolutionThe collected solid was dissolved into an organic solvent (chloroform/methanol=10/1)
6. washafter washing with water
7. dry with materialthe solution was dried over anhydrous magnesium sulfate
8. customThe solvent was evaporated
9. customthe resulting residue was triturated twice with chloroform