反応 #41346

反応方程式

isopentylnitrit

Acetic acid anhydride

2,5-dimethyl-4-iodoaniline

potassium acetate

→

subtitle compound

収率 21.0%

1-Acetyl-5-iodo-6-methylindazole

収率 21.0%

溶媒

benzene

反応条件

後処理

1. 1
   温度cooled
2. 2
   ろ過filtered
3. 3
   その他The filtrate was evaporated
4. 4
   その他purified by column chromatography (SiO2, dichloromethane)
5. 5
   workup.ADDITIONProduct containing fractions
6. 6
   濃縮concentrated

実験手順

Acetic acid anhydride (6.9 mL, 72 mmol) was added to a slurry of 2,5-dimethyl-4-iodoaniline (6.0 g, 24 mmol) and potassium acetate (2.4 g, 24 mmol) in benzene (50 mL). The mixture was heated to 80° C. and isopentylnitrit (4.8 mL, 36 mmol) was added during 20 min. The mixture was stirred at 80° C. overnight, then cooled and filtered. The filtrate was evaporated and purified by column chromatography (SiO2, dichloromethane). Product containing fractions were pooled and concentrated. The subtitle compound (1.5 g, 21%) was obtained as crystals from ethyl acetate.

出典