反应详情

温度

0 °C

1-(3-isopropyl-1,2,4-oxadiazol-5-yl)piperidin-4-ol (30 mg) was dissolved in N,N-dimethylformamide (2 mL) and cooled to an internal temperature of 0° C. Then, NaH (9 mg) was slowly added thereto and stirred for 30 min. 7-(2-fluoro-4-methanesulfonyl-phenyl)-4-methanesulfonyl-thieno[3,2-d]pyrimidine (50 mg) synthesized in Preparation Example 2 was slowly added thereto and heated to room temperature, followed by stirring for 2 hours. Then, the reaction mixture was mixed with a saturated solution of ammonium hydroxide, and extracted twice with ethyl acetate. The organic layer thus obtained was washed with water, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain a foamy residue. The residue was crystallized in the presence of diethyl ether to obtain the title compound (40 mg) as a whitish solid.

1. additionwas slowly added
2. temperatureheated to room temperature
3. stirringby stirring for 2 hours
4. extractionextracted twice with ethyl acetate
5. customThe organic layer thus obtained
6. washwas washed with water
7. dry with materialdried over anhydrous magnesium sulfate
8. concentrationconcentrated under reduced pressure
9. customto obtain a foamy residue
10. customThe residue was crystallized in the presence of diethyl ether