反应 #326990

ord-d7bab6e8aa57430bae35dab90d5c529d

反应方程式

NC1CCCCC1
cyclohexylamine
O=S1(=O)CCCCO1
1,4-butane sultone
O=S(=O)(O)CCCCNC1CCCCC1
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. 1
    温度The solution was heated
  2. 2
    温度to reflux for 2 hours
  3. 3
    过滤The solid was collected by filtration
  4. 4
    洗涤washed with acetone (2×20 mL)
  5. 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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08642801B2uspto-grants-2014_02