反应详情

温度

0 °C

Intermediate 370.2 (350 mg, 1.2 mmol) was dissolved in CH2Cl2 (10 mL) and Et3N (0.50 mL, 3.6 mmol) and cooled to 0° C., MsCl (0.092 mL, 1.2 mmol) was added dropwise and the mixture was stirred at 0° C. for 2 h. The reaction mixture was diluted with CH2Cl2 (20 mL), washed with H2O, brine, dried (Na2SO4) and concentrated to yield 370 mg of Intermediate 370.3 as a clear oil. 1H NMR (400 MHz, CDCl3) δ ppm 1.15 (t, J=7.58 Hz, 3H) 2.56 (q, 2H) 3.71 (s, 3H) 6.30 (s, 1H) 7.09-7.16 (m, 1H) 7.21-7.29 (m, 2H) 7.28-7.43 (m, 3H) 7.99-8.05 (m, 2H).

1. washwashed with H2O, brine
2. dry with materialdried (Na2SO4)
3. concentrationconcentrated