反应 #1563909

反应方程式

N-(6-iodobenzo[d][1,3]dioxol-5-yl)acetamide

NaOH

→

6-iodobenzo[d][1,3]dioxol-5-amine

收率 98.5%

溶剂

ethanol

water

反应条件

后处理

1. 1
   温度to reflux
2. 2
   温度The mixture was cooled
3. 3
   其他the solvent was removed under vacuum
4. 4
   其他The residue was partitioned between methylene chloride (100 mL) and water (100 mL)
5. 5
   洗涤The organic layer was washed with water (2×100 mL)
6. 6
   干燥dried (MgSO4)
7. 7
   其他evaporated under vacuum

实验过程

A solution of N-(6-iodobenzo[d][1,3]dioxol-5-yl)acetamide (200 mg, 0.656 mmol) and NaOH (1.31 g, 32.8 mmol) in ethanol (26 mL) and water (6 mL) was heated to reflux with stirring for 4 h. The mixture was cooled and the solvent was removed under vacuum. The residue was partitioned between methylene chloride (100 mL) and water (100 mL). The organic layer was washed with water (2×100 mL), dried (MgSO4) and evaporated under vacuum to give 6-iodobenzo[d][1,3]dioxol-5-amine (170 mg, 98%) as orange solid. LCMS: 264 [M+1]+; 1H NMR (DMSO-d6) δ 4.88 (s, 2H), 5.87 (s, 2H), 6.47 (s, 1H), 7.07 (s, 1H).

来源