反应 #792149

反应方程式

isopropylamine

3-methyl-2-nitrobenzoic acid

triethylamine

Ethyl chloroformate

→

desired intermediate

收率 80.2%

3-Methyl-N-(1-methylethyl)-2-nitrobenzamide

收率 80.2%

溶剂

methylene chloride

water

反应条件

后处理

1. 1
   其他a solid precipitate formed
2. 2
   workup.ADDITIONwas added
3. 3
   其他a homogeneous solution resulted
4. 4
   萃取extracted with ethyl acetate
5. 5
   洗涤The organic extracts were washed with water
6. 6
   干燥dried over magnesium sulfate
7. 7
   其他evaporated under reduced pressure

实验过程

A solution of 3-methyl-2-nitrobenzoic acid (2.00 g, 11.0 mmol) and triethylamine (1.22 g, 12.1 mmol) in 25 mL of methylene chloride was cooled to 10° C. Ethyl chloroformate was carefully added and a solid precipitate formed. After stirring for 30 minutes isopropylamine (0.94 g, 16.0 mmol) was added and a homogeneous solution resulted. The reaction was stirred for an additional hour, poured into water and extracted with ethyl acetate. The organic extracts were washed with water, dried over magnesium sulfate and evaporated under reduced pressure to afford 1.96 g of the desired intermediate as a white solid melting at 126-128° C.

来源