反应 #326979

反应方程式

EtOH

1,4-butanesultone

ethylamine

→

4-(ethylamino)-1-butanesulfonic acid

收率 75.0%

溶剂

acetone EtOH

tetrahydrofuran

反应条件

后处理

1. 1
   温度was warm up to room temperature
2. 2
   workup.STIRRINGThe reaction was stirred in these conditions overnight
3. 3
   workup.STIRRINGThe suspension was stirred for 5 minutes
4. 4
   过滤the solid was filtered
5. 5
   其他dried in vacuo

实验过程

A solution of 1,4-butanesultone (2.66 g, 18.6 mmol) in tetrahydrofuran (total volume: 4 mL) was added via syringe pump over a 4 hour period to ethylamine (70% w/w in water, 24 mL, 372 mmol) at 5° C. The solution was stirred at 5° C. for an additional 3 hours before it was warm up to room temperature. The reaction was stirred in these conditions overnight. The solvent was coevaporated with EtOH (1×25 mL). The solid was suspended in 50% acetone/EtOH (50 mL). The suspension was stirred for 5 minutes, the solid was filtered and dried in vacuo. Yield: 75%. 1H NMR (D2O, 500 MHz) δ ppm 2.95 (m, 4H), 2.82 (m, 2H), 1.68 (m, 4H), 1.13 (t, 3H, J=7.3 Hz), 1.14 (t, 3H, J=7.3 Hz). 13C (D2O, 125 MHz) δ ppm 50.27, 46.68, 42.99, 24.66, 21.48, 10.64. ES-MS182 (M+1).

来源