反应详情

In an oven-dried flask filled with N2 was added cyclopropanecarboxylic acid [(3-chloropyrazin-2-yl)-(4-phenoxyphenyl)-methyl]-amide (55 mg, 0.00014 mol), MeCN (4 mL, 0.07 mol) and DMF (0.7 mL, 0.009 mol). POCl3 was added dropwise at 0° C. The reaction mixture was warmed up to rt and stirred at that temperature overnight. The excess of POCl3 was removed under reduced pressure and the residue was quenched with solution of NH3 in i-PrOH (2 N) at 0° C. with vigorous stirring to adjust pH to 9. The crude reaction mixture was then charged with water and the aqueous layer was washed with DCM. The combined organic layer was dried over Na2SO4, filtered and concentrated under reduced pressure to give the title compound, which was used in next step without further purification.

1. customThe excess of POCl3 was removed under reduced pressure
2. customthe residue was quenched with solution of NH3 in i-PrOH (2 N) at 0° C.
3. stirringwith vigorous stirring
4. customThe crude reaction mixture
5. washthe aqueous layer was washed with DCM
6. dry with materialThe combined organic layer was dried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure