反应详情

温度

0 °C

Distilled triethyl amine (344 mL, 2.49 mol) was added slowly to a solution of compound of example 2 (350 g, 1.25 mol) in dry CH2Cl2 (2.5 L). To the reaction mixture methanesulfonyl chloride (122 mL, 171.1 g, 1.49 mol) was added with stirring, at 0° C., under an atmosphere of N2 and over a period of 20 min. The reaction mixture was further stirred for 1 h at 0° C. It was poured over saturated aqueous NaHCO3 solution (1.5 L). The organic layer was separated, washed with brine, dried (anhydrousNa2SO4) and concentrated to obtained a residue. This was dissolved in distilled isopropyl alcohol (1.5 L), anhydrous sodium acetate (408 g, 4.97 mmol) was added and the reaction mixture was refluxed for 1 h. It was cooled to room temperature. Sodium acetate was filtered off and washed with CHCl3. The filtrate was concentrated to obtain the title compound, which was purified using a silica gel column and 60% EtOAc+petroleum ether 60-80° C. as eluant.

1. stirringThe reaction mixture was further stirred for 1 h at 0° C
2. customThe organic layer was separated
3. washwashed with brine
4. customdried (anhydrousNa2SO4)
5. concentrationconcentrated
6. customto obtained a residue
7. temperaturethe reaction mixture was refluxed for 1 h
8. temperatureIt was cooled to room temperature
9. filtrationSodium acetate was filtered off
10. washwashed with CHCl3
11. concentrationThe filtrate was concentrated