反应详情

温度

-78 °C

1M BCl3 (0.46 mL, 0.468 mmol) was added to a solution of 3-benzyloxy-cyclobutanesulfonic acid [7-(2-fluoro-4-iodo-phenylamino)-6-methyl-5-oxo-2,3-dihydro-5H-thiazolo[3,2-a]pyridin-8-yl]-amide (0.1 g, 0.156 mmol) in dry DCM (3 mL) at −78° C. The resulting mixture was stirred at −78° C. for 3 hours. The reaction was monitored by TLC (10% MeOH in CHCl3). The reaction mixture was quenched with methanol, basified with saturated NaHCO3 solution and extracted with DCM. The organic layer was washed with brine, dried over Na2SO4 and concentrated. Purification by column chromatography on silica gel (4% MeOH in CHCl3), followed by preparative HPLC afforded 0.015 g of the product (18% yield).

1. customThe reaction mixture was quenched with methanol
2. extractionextracted with DCM
3. washThe organic layer was washed with brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customPurification by column chromatography on silica gel (4% MeOH in CHCl3)