反应 #1972083

反应方程式

3-Amino-6-chloro-2-hydroxy-benzenesulfonamide

2-ethylbutyric acid

DPPA

DMF

→

6-Chloro-3-[3-(1-ethyl-propyl)-ureido]-2-hydroxy-benzenesulfonamide

收率 15.0%

反应条件

后处理

1. 1
   温度the reaction heated at 70° C
2. 2
   workup.WAITAfter 18 hrs
3. 3
   其他the reaction mixture was quenched with water
4. 4
   萃取extracted with ethyl acetate
5. 5
   干燥The organic layers were dried over anhydrous magnesium sulfate
6. 6
   其他The crude residue was purified via HPLC

实验过程

To a solution of 2-ethylbutyric acid (0.125 mL, 1.0 mmol) in DMF (0.5 mL) was added DPPA (0.25 mL, 1.2 mmol) and TEA (0.25 mL, 1.8 mmol) and the reaction heated at 70° C. After 18 hrs, 3-Amino-6-chloro-2-hydroxy-benzenesulfonamide (1.0 mmol) was added and the reaction heated at 70° C. After 18 hrs, the reaction mixture was quenched with water and extracted with ethyl acetate. The organic layers were dried over anhydrous magnesium sulfate, and concentraed under reduced pressure. The crude residue was purified via HPLC to give 51 mg (15%) of 6-Chloro-3-[3-(1-ethyl-propyl)-ureido]-2-hydroxy-benzenesulfonamide. LC-MS (m/z) 336 (M+).

来源