反应详情

To a solution of the product of Example 39-6 (310 g, 0.705 mol) and pyridine (167.6 g, 2.12 mol) in dichloromethane (1645 mL) at 18-20° C. was added methanesulfonyl chloride (121.1 g, 1.06 mol) over 45 minutes. The solution was mixed at RT for 16 h then quenched with 1 M HCl (2000 mL). The layers were separated and the organic layer was concentrated under vacuum. The product was crystallized from ethyl acetate/heptane (1/1, 8 volumes) to give the title compound (236.0 g, 65%).

1. additionThe solution was mixed at RT for 16 h
2. customthen quenched with 1 M HCl (2000 mL)
3. customThe layers were separated
4. concentrationthe organic layer was concentrated under vacuum
5. customThe product was crystallized from ethyl acetate/heptane (1/1, 8 volumes)