反应详情

温度

4 °C

The product of Example 1 (59 g, 0.13 mol) was dissolved at room temperature in 120 mL of pyridine. The solution was put into an ice bath and 29 mL of methanesulfonyl chloride (0.34 mol) was added dropwise. The resulting solution was allowed to stir at 4° C. for 24 hours. The reaction mixture was added in three portions at a slow flow rate into a blender as described previously. The pea-green solid was collected by filtration, washed twice with 2 L of water, and dried to yield 58 g (93%). The compound started to soften at 85° C. and melted at 106-108° C. Rf =0.62 (CHCl3 --EtOH, 10:1). Anal. (C29H28N2O7S).

1. customThe solution was put into an ice bath
2. additionThe reaction mixture was added in three portions at a slow flow rate into a blender
3. filtrationThe pea-green solid was collected by filtration
4. washwashed twice with 2 L of water
5. customdried
6. customto yield 58 g (93%)
7. customto soften at 85° C.