反応 #46974

反応方程式

17

5-Bromo-1-(4-methoxy-benzenesulfonyl)-7-nitro-2,3-dihydro-1H-indole

ammonium chloride

water

→

compound 18

収率 89.0%

5-Bromo-1-(4-methoxy-benzenesulfonyl)-2,3-dihydro-1H-indol-7-yl amine

収率 89.0%

溶媒

isopropanol

反応条件

後処理

1. 1
   温度After cooling
2. 2
   ろ過the reaction mixture was filtrated
3. 3
   抽出extracted with CH2Cl2
4. 4
   乾燥The combined organic layer was dried by MgSO4
5. 5
   その他evaporated
6. 6
   その他to give a residue that
7. 7
   その他was purified by silica gel flash column chromatography (EtOAc:n-hexane=2:3)

実験手順

A mixture of 17 (9 g, 0.021 mol), iron (3.65 g, 0.065 mol), and ammonium chloride (2.33 g, 0.043 mol) in isopropanol (200 ml)-water (50 ml) was stirred at 100° C. for 4 h. After cooling, the reaction mixture was filtrated and extracted with CH2Cl2. The combined organic layer was dried by MgSO4 and evaporated to give a residue that was purified by silica gel flash column chromatography (EtOAc:n-hexane=2:3) to afford compound 18, yield 89%.

出典