反应详情

Solid KOH 6.80 g, (0.122 mol) and H2O (10 ml) are added to para-methoxyphenol 7.0 g (0.0564 mol), the resultant mixture is stirred at the room temperature while 3-chloropropanoic acid (6.12 g, 0.0564 mol) is added to thereof. Then the mixture is stirred and heated to reflux for 3 h. The reaction solution is acidified to pH 2 by adding concentrated aqueous HCl and extracted with ether. The combined ether extracts is then washed with 10% aqueous NaHCO3 and acidified to pH 3-4 by adding concentrated aqueous HCl, and precipitate is formed. The residue is filtered and recrystallized by benzene to provide needle crystal 2.0 g. m.p.: 102-103° C., yield: 18.1%.

1. additionis added to thereof
2. temperatureheated
3. temperatureto reflux for 3 h
4. extractionextracted with ether
5. washThe combined ether extracts is then washed with 10% aqueous NaHCO3
6. additionby adding concentrated aqueous HCl
7. customprecipitate is formed
8. filtrationThe residue is filtered
9. customrecrystallized by benzene