反应 #326990
ord-d7bab6e8aa57430bae35dab90d5c529d
反应方程式
cyclohexylamine
1,4-butane sultone
→
4-(cyclohexylamino)-1-butanesulfonic acid
收率 52.0%
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度The solution was heated
- 2温度to reflux for 2 hours
- 3过滤The solid was collected by filtration
- 4洗涤washed with acetone (2×20 mL)
- 5其他dried in vacuo
实验过程
To a solution of cyclohexylamine (2.0 g, 20.2 mmol) in 1,4-dioxane (13 mL) was added 1,4-butane sultone (2.61 g, 19.2 mmol). The solution was heated to reflux for 2 hours. The reaction was cooled to room temperature. The solid was collected by filtration, washed with acetone (2×20 mL) and dried in vacuo. Yield: 52%. 1H NMR (D2O, 500 MHz) δ ppm 2.95 (m, 3H), 2.81 (m, 2H), 1.92 (m, 2H), 1.67 (m, 6H), 1.52 (m, 1H), 1.18 (m, 4H), 1.02 (m, 1H). 13C (D2O, 125 MHz) δ ppm 57.32, 50.31, 44.01, 29.02, 24.84, 24.68, 24.07, 24.55. ES-MS 236 (M+1).