反応 #5470

反応方程式

HCl

sodium hydroxide

4-amino-5-chloro-2-[2-(diethylamino)-2-oxoethoxy]benzoic acid, methyl ester

methanol

→

fine colorless needles

収率 68.1%

4-Amino-5-chloro-2-[2-(diethylamino)-2-oxoethoxy]benzoic acid

収率 68.1%

溶媒

water

反応条件

後処理

1. 1
   その他formed (pH 3)
2. 2
   その他the solid was collected
3. 3
   洗浄washed with water, air
4. 4
   その他dried
5. 5
   その他recrystallized from 2-propanol

実験手順

A solution of 4-amino-5-chloro-2-[2-(diethylamino)-2-oxoethoxy]benzoic acid, methyl ester (7.87 g, 25 mmol) in water (70 g) containing methanol (40 g) was treated with 50% sodium hydroxide (10 g) and heated to 60° C. for 30 minutes. The mixture was neutralized with 3N HCl until a precipitate formed (pH 3), and the solid was collected, washed with water, air dried, and recrystallized from 2-propanol to afford (2 crops) 5.12 g (68%) of fine colorless needles; mp 186.5°-188.0° C.

出典