반응 #5468

반응 방정식

4-amino-5-chloro-2-(2-methoxyethoxy)benzoic acid methyl ester

sodium hydroxide

water

→

fine pale tan needles

수율 78.0%

4-Amino-5-chloro-2-(2-methoxyethoxy)benzoic acid

수율 78.0%

용매

ethanol

반응 조건

후처리

1. 1
   온도refluxed for one hour
2. 2
   기타The ethanol was removed in vacuo
3. 3
   추출The aqueous solution was extracted with ether (20 mL)
4. 4
   기타A solid soon precipitated
5. 5
   여과this was filtered
6. 6
   세척washed with water, air
7. 7
   기타dried
8. 8
   기타recrystallized from ethyl acetate (2 crops)

실험 절차

A solution of 4-amino-5-chloro-2-(2-methoxyethoxy)benzoic acid methyl ester (2.75 g, 10.6 mmol) in 95% ethanol (20 mL) was treated with 50% sodium hydroxide (10 mL) and water (10 mL), and refluxed for one hour. The ethanol was removed in vacuo and replaced with water. The aqueous solution was extracted with ether (20 mL) and acidified to pH 4 with concentrated hydrochloric acid (16 mL). A solid soon precipitated, and this was filtered, washed with water, air dried, and recrystallized from ethyl acetate (2 crops) to afford 2.03 g (75%) of fine pale tan needles; mp 119°-120° C.

출처