反応 #2017438

反応方程式

Methyl 3-tert-butyl-2-methoxy-5-nitrobenzoate

ammonium chloride

water

→

title compound

収率 100.0%

methyl 5-amino-3-tert-butyl-2-methoxybenzoate

収率 100.0%

溶媒

methanol

反応条件

後処理

1. 1
   ろ過filtered through celite
2. 2
   洗浄the celite washed with methanol
3. 3
   濃縮The filtrate was then concentrated under vacuum
4. 4
   workup.DISSOLUTIONdissolved in ethyl acetate (600 mL)
5. 5
   洗浄The resultant solution was then washed with water and brine
6. 6
   抽出The organic extract
7. 7
   その他was then dried
8. 8
   ろ過filtered
9. 9
   濃縮concentrated under vacuum

実験手順

Methyl 3-tert-butyl-2-methoxy-5-nitrobenzoate (10.42 g, 39.0 mmol), iron powder (325 mesh, 10.89 g, 195 mmol), ammonium chloride (3.13 g, 58.5 mmol), water (30 mL), and methanol (150 mL) were added together. The resultant mixture was then refluxed for 1 h. The mixture was then cooled to room temperature, filtered through celite, and the celite washed with methanol. The filtrate was then concentrated under vacuum and dissolved in ethyl acetate (600 mL). The resultant solution was then washed with water and brine. The organic extract was then dried, filtered and concentrated under vacuum to yield the title compound as an oil (9.25 g, 100%).

出典