反応 #2286288

反応方程式

[3-chloro-4-(6-chloro-5-isopropyl-pyridazin-3-yloxy)-5-methyl-phenyl]-acetic acid methyl ester

[3-Chloro-4-(6-chloro-5-isopropyl-pyridazin-3-yloxy)-5-methyl-phenyl]-acetic acid methyl ester

sodium hydroxide

→

[3-chloro-4-(6-chloro-5-isopropyl-pyridazin-3-yloxy)-5-methyl-phenyl]-acetic acid

収率 100.0%

[3-Chloro-4-(6-chloro-5-isopropyl-pyridazin-3-yloxy)-5-methyl-phenyl]-acetic acid

収率 100.0%

溶媒

methanol

反応条件

後処理

1. 1
   濃縮At this time, the reaction mixture was concentrated under vacuum
2. 2
   workup.ADDITIONThe resulting solid was diluted with water and ethyl acetate
3. 3
   workup.ADDITIONThe water layer was acidified by the addition of a 1N aqueous hydrochloric acid solution
4. 4
   抽出was extracted with ethyl acetate
5. 5
   洗浄The organic layers were washed with a saturated aqueous sodium chloride solution
6. 6
   乾燥dried with magnesium sulfate
7. 7
   ろ過filtered
8. 8
   濃縮concentrated under vacuum

実験手順

A solution of [3-chloro-4-(6-chloro-5-isopropyl-pyridazin-3-yloxy)-5-methyl-phenyl]-acetic acid methyl ester (8b) (1.1 g, 2.97 mmol) in methanol (30 mL) at room temperature was treated dropwise with a 1N aqueous sodium hydroxide solution (5.9 mL, 5.9 mmol). The reaction was stirred at room temperature for 4 d. At this time, the reaction mixture was concentrated under vacuum. The resulting solid was diluted with water and ethyl acetate. The ethyl acetate layer was discarded. The water layer was acidified by the addition of a 1N aqueous hydrochloric acid solution and was extracted with ethyl acetate. The organic layers were washed with a saturated aqueous sodium chloride solution, dried with magnesium sulfate, filtered and concentrated under vacuum to afford [3-chloro-4-(6-chloro-5-isopropyl-pyridazin-3-yloxy)-5-methyl-phenyl]-acetic acid (9b) (1.05 g, 100%) as a white solid. This material was used without further purification; EI(+)-HRMS m/z calcd for C16H16Cl2N2O3 (M+) 355.0611, found 355.0610. Molecular Weight=355.2235; Exact Mass=354.0538

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