Diethylamine → N,N-Diethyl-2,2-difluoroacetamide
Reaction equation
[CH2:1]([NH:3][CH2:4][CH3:5])[CH3:2].C(N(CC)CC)C.C([O:15][C:16](F)(F)[CH:17]([F:19])[F:18])C>C(Cl)Cl>[CH2:1]([N:3]([CH2:4][CH3:5])[C:16](=[O:15])[CH:17]([F:18])[F:19])[CH3:2]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
The crude reaction gas was bubbled at 10° C. in a 2 l plastic bottle charged with 219 g (3.0 mols) of diethylamine, 303 g (3.0 mols) of triethylamine and 300 g of methylene chloride. Then, 365 g (2.5 mols) of 1-ethoxy-1,1,2,2-tetrafluoroethane was fed over a period of about 75 minutes. Then, nitrogen was supplied to the gas phase reactor at a rate of 200 cc/min for 20 minutes. The crude reaction solution was washed with 2 l of water, and the aqueous phase was extracted with 300 g of methylene chloride. The organic layers were put together and distilled to obtain 353 g (yield: 93.5%) of N,N-diethyl difluoroacetic acid amide (boiling point: 64° C./11 torr) having a purity of at least 99.5%.
Workup
- customThe crude reaction gas
- customwas bubbled at 10° C. in a 2 l plastic bottle
- customThe crude reaction solution
- washwas washed with 2 l of water
- extractionthe aqueous phase was extracted with 300 g of methylene chloride
- distillationdistilled
Sources & evidence
- ORD record
- ord-dfeb90f8555a4389a19c6f505bdafd3e
- Source dataset
- uspto-grants-1998_01
- Patent number
- US05710317
Reaction notes
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