反応 #11511

反応方程式

Methyl 4-aminobenzoate

iodine

→

Methyl 4-amino-3-iodobenzoate

溶媒

ethanol

反応条件

後処理

1. 1
   ろ過filtered over Celite
2. 2
   その他the filtrate was evaporated to dryness under reduced pressure
3. 3
   その他The residue was chromatographed on silica gel (230–400 mesh)
4. 4
   洗浄eluted with 1% ethyl acetate in hexane
5. 5
   その他to give 35 g (63%)

実験手順

Methyl 4-aminobenzoate (30.23 g, 200 mmol) was added to a mixture of iodine (60.91 g, 240 mmol) and silver sulfate (81.07 g, 260 mmol) in 1 L of ethanol at room temperature. The mixture was stirred at room temperature for 18 hours, filtered over Celite and the filtrate was evaporated to dryness under reduced pressure. The residue was chromatographed on silica gel (230–400 mesh) and eluted with 1% ethyl acetate in hexane to give 35 g (63%).

出典