반응 #1563909

반응 방정식

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

NaOH

→

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

수율 98.5%

용매

ethanol

water

반응 조건

후처리

1. 1
   온도to reflux
2. 2
   온도The mixture was cooled
3. 3
   기타the solvent was removed under vacuum
4. 4
   기타The residue was partitioned between methylene chloride (100 mL) and water (100 mL)
5. 5
   세척The organic layer was washed with water (2×100 mL)
6. 6
   건조dried (MgSO4)
7. 7
   기타evaporated under vacuum

실험 절차

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).

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