Reaktion #710459

Reaktionsgleichung

sulfuric acid

2-amino-3,5-dichlorobenzoic acid

sulfuric acid

methanol

→

2-amino-3,5-dichlorobenzoic acid methyl ester

Ausbeute 78.6%

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added twice),
2. 2
   Temperaturafter cooling most of the solvent
3. 3
   Sonstigewas removed under reduced pressure, and 300 mL of water
4. 4
   workup.ADDITIONwas added
5. 5
   Extraktionextracted with 200 mL of ethyl acetate
6. 6
   Waschenwashed with water for one time
7. 7
   Trocknendried over anhydrous sodium sulfate
8. 8
   Filtrationfiltered
9. 9
   Sonstigethe solvent was remove

Vorschrift

To a 500 mL round-bottom flask, 0.2 mol of 2-amino-3,5-dichlorobenzoic acid having a structural formula of IV-4, 300 mL of methanol, and 5 mL of concentrated sulfuric acid were added, heated to 64° C. and reacted for 12 hours (into which 3 mL of concentrated sulfuric acid was added twice), after cooling most of the solvent was removed under reduced pressure, and 300 mL of water was added, the pH was adjusted to 9-10 with a saturated sodium hydroxide solution, extracted with 200 mL of ethyl acetate, washed with water for one time, dried over anhydrous sodium sulfate, filtered and the solvent was remove to obtain a crude product, 34.6 grams of 2-amino-3,5-dichlorobenzoic acid methyl ester having a structure as shown by VIII-1 was obtained by column chromatography, and the yield was 78.6%;

Quelle