反応 #90258

反応方程式

water

3,4-dimethoxy-5-nitrobenzoic acid

2-Trifluoromethyl-nicotinic acid hydrazide

→

2-trifluoromethyl-nicotinic acid N′-(3,4-dimethoxy-5-nitro-benzoyl)-hydrazide

収率 73.2%

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   温度at reflux for three hours
2. 2
   温度at reflux overnight
3. 3
   温度to cool to room temperature
4. 4
   ろ過the copious precipitate was filtered off
5. 5
   洗浄washed with water
6. 6
   その他dried

実験手順

A mixture of 3,4-dimethoxy-5-nitrobenzoic acid (0.53 g, 2.34 mmol) and 1,1-carbonyldiimidazole (0.42 g, 2.59 mmol) was heated in tetrahydrofuran (10 mL) at reflux for three hours and then cooled to room temperature. 2-Trifluoromethyl-nicotinic acid hydrazide (0.53 g, 2.57 mmol) was added in one portion and the yellowish mixture was stirred at reflux overnight and then allowed to cool to room temperature. The mixture was poured onto cold water (100 mL) and the copious precipitate was filtered off, washed with water and dried to give 2-trifluoromethyl-nicotinic acid N′-(3,4-dimethoxy-5-nitro-benzoyl)-hydrazide (0.71 g, 73%).

出典