تفاعل #939048

معادلة التفاعل

3-amino-2-chlorobenzoic acid

sulfuric acid

methanol

→

desired compound

المردود 92.0%

Methyl 3-amino-2-chlorobenzoate

المردود 92.0%

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas heated
2. 2
   درجة الحرارةunder reflux for 24 hours
3. 3
   workup.DISTILLATIONto distill the solvent off
4. 4
   workup.ADDITIONThe residue was neutralized by addition of aqueous saturated sodium hydrogen carbonate
5. 5
   استخلاصThe neutralized mixture was extracted with toluene
6. 6
   تجفيفdried over anhydrous magnesium sulfate
7. 7
   workup.DISTILLATIONto distill the solvent off

الإجراء التجريبي

A mixture of 3-amino-2-chlorobenzoic acid (500 mg, 2.91 mmol), conc. sulfuric acid (6 mL), and methanol (150 mL) was heated under reflux for 24 hours, and placed under reduced pressure to distill the solvent off. The residue was neutralized by addition of aqueous saturated sodium hydrogen carbonate. The neutralized mixture was extracted with toluene, dried over anhydrous magnesium sulfate, and placed under reduced pressure to distill the solvent off. There was obtained 497 mg (yield 92%) of the desired compound in the form of pale brown oil.

المصدر