반응 #792149

반응 방정식

isopropylamine

3-methyl-2-nitrobenzoic acid

triethylamine

Ethyl chloroformate

→

desired intermediate

수율 80.2%

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

수율 80.2%

용매

methylene chloride

water

반응 조건

후처리

1. 1
   기타a solid precipitate formed
2. 2
   workup.ADDITIONwas added
3. 3
   기타a homogeneous solution resulted
4. 4
   추출extracted with ethyl acetate
5. 5
   세척The organic extracts were washed with water
6. 6
   건조dried over magnesium sulfate
7. 7
   기타evaporated under reduced pressure

실험 절차

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.

출처