تفاعل #792149

معادلة التفاعل

isopropylamine

3-methyl-2-nitrobenzoic acid

triethylamine

Ethyl chloroformate

→

desired intermediate

المردود 80.2%

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

المردود 80.2%

المذيبات

methylene chloride

water

ظروف التفاعل

المعالجة

1. 1
   أخرىa solid precipitate formed
2. 2
   workup.ADDITIONwas added
3. 3
   أخرىa homogeneous solution resulted
4. 4
   استخلاصextracted with ethyl acetate
5. 5
   غسيلThe organic extracts were washed with water
6. 6
   تجفيفdried over magnesium sulfate
7. 7
   أخرىevaporated under reduced pressure

الإجراء التجريبي

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.

المصدر