反应详情

A mixture of N-{4-methyl-5-[2-(1-methyl-cyclopropyl)-pyridin-4-yl]-thiazol-2-yl}-acetamide (Step 1.3) (34.8 mmol), a 6N aqueous solution of HCl (53 mL) and EtOH (265 mL) was stirred for 5 h at 85° C., cooled to rt and then concentrated. The residue was slowly diluted with a saturated solution of NaHCO3 and then extracted with EtOAc (3×). The combined organic phases were successively washed with a saturated solution of NaHCO3 and brine, dried (Na2SO4), filtered and concentrated. The residue was triturated with CH2Cl2 and then filtered to afford the title compound as a yellow-green solid. HPLC: t=3.55 min (method B); LC-MS: tR=1.03 min, [M+H]+ 246; TLC: Rf=0.26 (1:2 Hex/EtOAc).

1. concentrationconcentrated
2. additionThe residue was slowly diluted with a saturated solution of NaHCO3
3. extractionextracted with EtOAc (3×)
4. washThe combined organic phases were successively washed with a saturated solution of NaHCO3 and brine
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was triturated with CH2Cl2
9. filtrationfiltered