Water → (2S)-3,3,3-Trifluoro-2-methylpropane-1,2-diamine
Reaction equation
Cl.[F:2][C:3]([F:10])([F:9])[C@@:4]([CH3:8])([NH2:7])[CH2:5][NH2:6].O>C(OCC)C>[F:2][C:3]([F:10])([F:9])[C@@:4]([CH3:8])([NH2:7])[CH2:5][NH2:6]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
Into a flask, are introduced 4.8 g of (2S)-3,3,3-trifluoro-2-methyl-propane-1,2-diamine hydrochloride, 2.5 mL of water and 100 mL of ethyl ether. 4.5 mL of 32% soda are added dropwise on the resulting mixture until pH=12. The aqueous phase is then decanted and then extracted 4 times with 200 mL of ethyl ether. The organic phases are collected, dried on magnesium sulfate, filtered and then concentrated under reduced pressure (300 mbars/bath temperature=25° C.) in order to obtain 2.3 g of (2S)-3,3,3-trifluoro-2-methyl-propane-1,2-diamine, as a pale yellow oil, including the following characteristics:
Workup
- addition4.5 mL of 32% soda are added dropwise on the resulting mixture until pH=12
- customThe aqueous phase is then decanted
- extractionextracted 4 times with 200 mL of ethyl ether
- customThe organic phases are collected
- customdried on magnesium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure (300 mbars/bath temperature=25° C.) in order
Sources & evidence
- ORD record
- ord-0998f1504fe74eaabb79b01bc71f1179
- Source dataset
- uspto-grants-2014_08
- Patent number
- US08815853B2
Reaction notes
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