反応 #47827

反応方程式

6-Methoxy-1-oxo-3-phenyl-1H-indene-2-carboxylic acid ethyl ester

hydroxylamine hydrochloride

pyridine

→

titled compound

収率 80.0%

1-hydroxyimino-6-methoxy-3-phenyl-1H-indene-2-carboxylic Acid Ethyl Ester

収率 80.0%

溶媒

ethanol

反応条件

後処理

1. 1
   温度refluxed for 1 hr
2. 2
   洗浄The resulting mixture washed with saturated sodium bicarbonate
3. 3
   抽出extracted with ethyl acetate
4. 4
   その他The organic layer was separated
5. 5
   乾燥dried over anhydrous MgSO4
6. 6
   濃縮concentrated under a reduced pressure
7. 7
   その他The resulting residue was purified by flash chromatography

実験手順

6-Methoxy-1-oxo-3-phenyl-1H-indene-2-carboxylic acid ethyl ester (1.6 g, 5.19 mmol) obtained in Example 1 was dissolved in ethanol (100 mL), hydroxylamine hydrochloride (1.08 g, 15.57 mmol) and pyridine (1.64 g, 1.68 mL, 20.76 mmol) were added thereto, refluxed for 1 hr, and cooled to RT. The resulting mixture washed with saturated sodium bicarbonate and extracted with ethyl acetate. The organic layer was separated, dried over anhydrous MgSO4 and concentrated under a reduced pressure. The resulting residue was purified by flash chromatography to obtain 1.34 g of the titled compound (yield: 80%).

出典