反応 #70947

反応方程式

3,4-dimethoxy-N-methyl-5-nitro-benzamide

phosphorous pentachloride

→

3,4-dimethoxy-N-methyl-5-nitro-benzimidoyl chloride

溶媒

toluene

反応条件

後処理

1. 1
   workup.ADDITIONUpon completion of addition
2. 2
   温度the reaction mixture was warmed
3. 3
   温度to reflux till complete disappearance of starting material
4. 4
   その他Evaporation to dryness
5. 5
   その他resulted in a crude solid
6. 6
   洗浄that was washed with diethyl ether

実験手順

To a stirred suspension of 3,4-dimethoxy-N-methyl-5-nitro-benzamide (0.40 g, 1.66 mmol) in toluene (10 mL) was added phosphorous pentachloride (0.28 g, 1.83 mmol) portionwise. Upon completion of addition, the reaction mixture was warmed to reflux till complete disappearance of starting material. Evaporation to dryness resulted in a crude solid that was washed with diethyl ether, affording 3,4-dimethoxy-N-methyl-5-nitro-benzimidoyl chloride, 0.37 g (85%).

出典