反应详情

温度

110 °C

A 5 ml micro wave vial was charged with 3-chloro-5-(4-(4-methoxyphenethyl)piperazin-1-yl)-1,2,4-thiadiazole (50 mg, 148 μmol) in 3 mL DME. 4-Cyanophenylboronic acid (26.0 mg, 177 μmol), Na2CO3 (18.8 mg, 177 μmol), tetrakis(triphenylphosphine) palladium (0) (3.41 mg, 2.95 μmol) and water (1.5 mL) was added. The vial was capped and the mixture was heated in oil bath at 110° C. over night. 2 mL EtOAc were added and the aqueous part was separated. The organic layer was dried over Na2SO4, filtered off and concentrated in vacuo. The crude product was dissolved in MeCN (3 mL)/DIPEA (100 μL) and purified by preparative HPLC on reversed phase eluting with a gradient formed from MeCN, water and NEt3 to yield, after evaporation of the product containing fractions, 13.6 mg (23%) of the title compound as white solid. MS (m/e): 406.3 (MH+).

1. customThe vial was capped
2. customthe aqueous part was separated
3. dry with materialThe organic layer was dried over Na2SO4
4. filtrationfiltered off
5. concentrationconcentrated in vacuo
6. dissolutionThe crude product was dissolved in MeCN (3 mL)/DIPEA (100 μL)
7. custompurified by preparative HPLC on reversed phase
8. washeluting with a gradient
9. customformed from MeCN, water and NEt3
10. customto yield
11. customafter evaporation of the product
12. additioncontaining fractions, 13.6 mg (23%) of the title compound as white solid