反应详情

Mesyl anhydride (430 mg, 2.46 mmol) was added portionwise to a solution of 36B (470 mg, 2.05 mmol) in CH2Cl2 (10 mL) and Et3N (0.57 mL, 4.1 mmol) at 0° C. After stirring for 15 h at ambient temperature, the mixture was diluted with CH2Cl2 (80 mL), washed with 1.0 M HCl, NaHCO3, brine, dried over Na2SO4 and concentrated in vacuo. The crude mesylate was dissolved in EtOAc (20 mL) and methyl amine (33%, 5 mL) and heated in a pressure tube for 2 h. The reaction mixture was concentrated in vacuo to afford 36C (500 mg, 99%) as a yellow oil. MS (ESI) m/z 242.0/244.0 (M+H)+.

1. washwashed with 1.0 M HCl, NaHCO3, brine
2. dry with materialdried over Na2SO4
3. concentrationconcentrated in vacuo
4. dissolutionThe crude mesylate was dissolved in EtOAc (20 mL)
5. temperaturemethyl amine (33%, 5 mL) and heated in a pressure tube for 2 h
6. concentrationThe reaction mixture was concentrated in vacuo