تفاعل #5468

معادلة التفاعل

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

sodium hydroxide

water

→

fine pale tan needles

المردود 78.0%

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

المردود 78.0%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةrefluxed for one hour
2. 2
   أخرىThe ethanol was removed in vacuo
3. 3
   استخلاصThe aqueous solution was extracted with ether (20 mL)
4. 4
   أخرىA solid soon precipitated
5. 5
   ترشيحthis was filtered
6. 6
   غسيلwashed with water, air
7. 7
   أخرىdried
8. 8
   أخرىrecrystallized from ethyl acetate (2 crops)

الإجراء التجريبي

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.

المصدر