反应详情

Ethyl thioglycolate (73 μL, 0.66 mmol) was added to a solution of {2-[5-(4-fluorophenylcarbamoyl)-2-methylsulfonyl-pyrimidin-4-ylamino]-ethyl}carbamic acid tert-butyl ester (0.30 g, 0.66 mmol) and DIPEA (117 μL, 0.66 mmol) in DMF (1.5 mL). The resulting solution was stirred under N2 overnight. The reaction mixture was then diluted with ethyl acetate (20 mL) and washed with water (10 mL), 1 N HCl (3×10 mL), water (10 mL), saturated NaHCO3 (3×10 mL), water (10 mL), saturated NaCl (20 mL) and dried over MgSO4. Following filtration, the solvent was removed by rotary evaporation to yield the titled product (0.19 g, 58%) as an off-white solid. 1H NMR: (d6-DMSO) δ 10.25 (s, 1H), 8.63 (m, 1H), 8.57 (s, 1H), 7.65 (m, 2H), 7.16 (m, 2H), 6.91 (t, 1H), 4.08 (q, 2H), 3.96 (s, 2H), 3.44 (m, 2H), 3.08 (m, 2H), 1.31 (s, 9H), 1.16 (t, 3H); HPLC: Rt=4.41 min; MS (ESI): m/z 492.44 (M−H)−.

1. washwashed with water (10 mL), 1 N HCl (3×10 mL), water (10 mL), saturated NaHCO3 (3×10 mL), water (10 mL), saturated NaCl (20 mL)
2. dry with materialdried over MgSO4
3. filtrationfiltration
4. customthe solvent was removed by rotary evaporation