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ChemicalBook CAS DataBase List D-2-AMINO-1,1,1-TRIFLUORO-3-(METHYL)BUTANE
1582-18-9

D-2-AMINO-1,1,1-TRIFLUORO-3-(METHYL)BUTANE synthesis

3synthesis methods
-

Yield:-

Reaction Conditions:

with hydrogen in methanol at 90; under 1500.15 Torr;Autoclave;Large scale;

Steps:

General procedure
General procedure: An autoclave was charged with 3 Kg of the oxime obtained above, 0.1 Kg of Raney nickel (moisturized with methanol) and 30 L of methanol. The autoclave was pressurized with hydrogen at a pressure of 0.2 MPa and heated to 90 °C. After hydrogen was consumed completely, the reaction mixture was cooled to room temperature and filtered. The filtrate was cooled down and acidified with diluted hydrochloric acid. The acidified solution was evaporated and the obtained solid was washed with diethylether and dried to yield 2-amino-1,1,1-trifluoropropane hydrochloride. Hydrochloride obtained above was placed in a three necked flask with stirrer, dropping funnel and condenser.The oil bath was heated up to 90 °C and an aqueous sodium hydroxide solution was slowly added to the flask. The liberated amine was collected by distillation with a boiling point of 46-47 °C (98 % yield).

References:

Jiang;Cheng;Yuan [Asian Journal of Chemistry,2015,vol. 27,# 7,p. 2406 - 2408]

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