Реакция #78098

Уравнение реакции

methyl 4-chloro-3-nitrobenzoate

2d

3-(1-acetylpiperazin-4-yl)aniline

triethylamine

→

methyl 4-(3-(1-acetylpiperazin-4-yl)anilino)-3-nitrobenzoate

Выход 85.0%

Растворители

NMP

Условия реакции

Обработка

1. 1
   ТемператураThe mixture was heated
2. 2
   Экстракцияthe resulting mixture was extracted with ethyl acetate (3×10 ml)
3. 3
   ПромывкаThe combined organic extracts were washed with water
4. 4
   Сушкаdried over sodium sulfate
5. 5
   Другоеevaporated to dryness
6. 6
   ДругоеThe residue was triturated with petroleum ether

Методика

To a solution of methyl 4-chloro-3-nitrobenzoate (2.0 g, 9.28 mmol) in anhydrous NMP (5 ml) was added 2d (2.03 g, 9.28 mmol) and triethylamine (1.3 ml, 9.28 mmol). The mixture was heated with stirring to 80° C. overnight. The cooled solution was poured into ice-water (50 ml) and the resulting mixture was extracted with ethyl acetate (3×10 ml). The combined organic extracts were washed with water, dried over sodium sulfate and evaporated to dryness. The residue was triturated with petroleum ether to yield methyl 4-(3-(1-acetylpiperazin-4-yl)anilino)-3-nitrobenzoate (3.14 g, 85%) as red crystals.

Источник