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Disperse 5.1 g (30.5 mmol) of chloral hydrate in 100 mL of water.Add 35.1 g (247.1 mmol) of anhydrous sodium sulfate, heat to 35 C in an oil bath, stir to dissolve,4.7 g (27.7 mmol) of <strong>[70146-15-5]1-aminoindan hydrochloride</strong> was added in one portion.A mixed solution of 6.1 g (88.1 mmol) of hydroxylamine hydrochloride and 30 mL of water was heated to 90 C, and the mixture was stirred for 8 hours, then cooled to room temperature, filtered, and the filter cake was washed with water and dried to give 4.7 g of a yellow solid.The yellow solid obtained above was added to 50 mL of 86% sulfuric acid at 60 C, the temperature was controlled at 60-65 C, the reaction was stirred for 30 minutes, the temperature was raised to 80 C, the reaction was stirred for 30 minutes, cooled to room temperature, and the reaction solution was poured. In 500 mL of ice water, the mixture was filtered, and the filter cake was washed with water and dried to give 2.3 g of compound int.
Multi-step reaction with 3 steps
1.1: sodium hydroxide / water; dichloromethane / Large scale
2.1: potassium carbonate / acetonitrile / 24 h / 60 - 70 °C / Large scale
2.2: 30 min / 50 - 80 °C / Large scale
3.1: sodium hydroxide / water; dichloromethane / > 10 min / Large scale
3.2: 30 min / 50 - 80 °C / Large scale
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