反应 #326977

ord-64e760af991a4103ae876b81f37a9664

反应方程式

CC(C)(C)N
tert-butylamine
O=S1(=O)CCCCO1
1,4-butane sultone
CC(C)(C)NCCCCS(=O)(=O)O
4-(tert-butylamino)-1-butanesulfonic acid

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度at reflux for 2 hours
  2. 2
    过滤The solid was collected by filtration
  3. 3
    洗涤washed with acetone (2×20 mL)
  4. 4
    其他dried in vacuo

实验过程

To a solution of tert-butylamine (1.0 mL, 9.5 mmol) in tetrahydrofuran (4 mL) was added 1,4-butane sultone (1.36 g, 10.0 mmol) at room temperature. The solution was stirred at 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: 690 mg (34%). 1H NMR (D2O, 500 MHz) δ ppm 2.92 (t, 2H, J=7.1 Hz), 2.82 (t, 2H, J=7.1 Hz), 1.68 (m, 4H), 1.22 (s, 9H). 13C (D2O, 125 MHz) δ ppm 57.07, 50.30, 40.95, 25.28, 24.96, 21.62. ES-MS 210 (M−1).

来源

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