تفاعل #939039

معادلة التفاعل

4-Hydroxy-3-nitrobenzoic acid

sulfuric acid

methanol

→

desired compound

المردود 58.0%

Methyl 4-hydroxy-3-nitrobenzoate

المردود 58.0%

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe suspension was heated overnight
2. 2
   درجة الحرارةunder reflux
3. 3
   workup.DISTILLATIONThe methanol was distilled off under reduced pressure
4. 4
   workup.DISSOLUTIONThe residue was dissolved in ethyl acetate (40 mL)
5. 5
   غسيلwashed successively with aqueous sodium hydrogen carbonate (20 mL×2) and saturated aqueous brine (20 mL)
6. 6
   تجفيفdried over anhydrous sodium sulfate
7. 7
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure

الإجراء التجريبي

4-Hydroxy-3-nitrobenzoic acid (10.0 g, 54.6 mmol) was suspended in methanol (60 mL). After addition of conc. sulfuric acid (0.1 mL), the suspension was heated overnight under reflux. The methanol was distilled off under reduced pressure. The residue was dissolved in ethyl acetate (40 mL), washed successively with aqueous sodium hydrogen carbonate (20 mL×2) and saturated aqueous brine (20 mL), and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, to give 6.27 g (yield 58%) of the desired compound in the form of a pale brown crystalline product.

المصدر