反应详情

温度

45 °C

N,N,N′,N′-Tetramethyl-1,3-propanediamine (56.7 g) was added dropwise to a suspension of the product from step (ii) (85.0 g) and 2,4,6-trimethylbenzenesulfonyl chloride (87.8 g) in THF (452.9 g), and the mixture was heated at 45° C. for 7 hours. 2.5% HCl in water (1291 g) was added to the mixture, and the mixture was stirred at 5° C. for 30 minutes. The resulting precipitate was collected by filtration, washed with acetonitrile (2×68.0 g), and dried to give the crude subtitle compound as a solid. A stirred suspension of the solid in acetonitrile (654.5 g) was heated at 70° C. for 30 minutes, cooled to 5° C. and stirred at 5° C. for 30 minutes. The resulting precipitate was collected by filtration, washed with acetonitrile (2×68.0 g) and dried to give the subtitle compound as a solid, 113.1 g; 1H NMR CDCl3: δ 7.24 (d, 2H), 7.11 (d, 2H), 6.96 (s, 2H), 4.71 (s, 2H), 3.90 (s, 2H), 3.71 (s, 2H), 2.59 (s, 6H), 2.32 (s, 3H), 2.27 (s, 3H).

1. filtrationThe resulting precipitate was collected by filtration
2. washwashed with acetonitrile (2×68.0 g)
3. customdried
4. customto give the crude subtitle compound as a solid
5. temperaturewas heated at 70° C. for 30 minutes
6. temperaturecooled to 5° C.
7. stirringstirred at 5° C. for 30 minutes
8. filtrationThe resulting precipitate was collected by filtration
9. washwashed with acetonitrile (2×68.0 g)
10. customdried