反应详情

A solution of 3-[6-amino-5-(1,3-benzothiazol-2-yl)pyridin-3-yl]phenol (80 mg, 0.20 mmol), potassium carbonate (100 mg, 0.700 mmol) and chloroacetic acid methyl ester (33 mg, 0.30 mmol) in DMF was left to stir at rt overnight. To the mixture was added EtOAc (10 mL), which was left to stir at rt for 10 min. Then, the mixture was washed with NaHCO3 aq. soln. (2×). The combined organic extracts were treated with brine, dried over anhydrous Na2SO4 and concentrated in vacuo. Purification via silica gel chromatography (5% MeOH in DCM) afforded the title compound as a yellow solid. MS (ES+): m/z=392.02 (100) [MH+]. HPLC: tR=3.63 min (ZQ3, polar—5 min).

1. waitwas left
2. stirringto stir at rt for 10 min
3. washThen, the mixture was washed with NaHCO3 aq. soln
4. additionThe combined organic extracts were treated with brine
5. dry with materialdried over anhydrous Na2SO4
6. concentrationconcentrated in vacuo
7. customPurification via silica gel chromatography (5% MeOH in DCM)