反应 #989758

反应方程式

4-hydrazino-2-methyltetrahydropyran hydrochloride

hydrochloric acid

( 1 )

4-hydrazino-2-methyltetrahydropyran hydrochloride

ethanol

sodium hydroxide

→

4-amino-2-methyltetrahydropyran hydrochloride

收率 64.3%

溶剂

n-butyl alcohol

water

反应条件

后处理

1. 1
   其他To a flask having
2. 2
   其他equipped with a stirring device
3. 3
   其他the mixture was reacted at 75° C. for 24 hours under hydrogen atmosphere
4. 4
   其他After completion of the reaction
5. 5
   过滤filtered
6. 6
   浓缩the filtrate was concentrated under reduced pressure
7. 7
   浓缩the resulting mixture was concentrated under reduced pressure

实验过程

To a flask having an inner volume of 500 ml, made of glass and equipped with a stirring device, a thermometer and a reflux condenser were charged 65.3 g (392 mmol) of 4-hydrazino-2-methyltetrahydropyran hydrochloride with a purity of 100% and synthesized in the same manner as in the above-mentioned (1), 18.0 g of developed Raney nickel, 120 ml of ethanol, 120 ml of water and 40 ml (320 mmol) of 8 mol/l aqueous sodium hydroxide solution, and the mixture was reacted at 75° C. for 24 hours under hydrogen atmosphere. After completion of the reaction, the reaction mixture was cooled to room temperature and filtered, and the filtrate was concentrated under reduced pressure. Then, 200 ml of n-butyl alcohol and 50 ml (600 mmol) of 12 mol/l hydrochloric acid were added to the concentrate, the resulting mixture was concentrated under reduced pressure to obtain 38.2 g (Isolation yield: 63%) of 4-amino-2-methyltetrahydropyran hydrochloride with a purity of 98% (areal percentage by gas chromatography) as white powder.

来源