3-Aminopyrrolidine → HCID 14836607, compound
Reaction equation
[NH2:1][CH:2]1[CH2:6][CH2:5][NH:4][CH2:3]1.[F:7][C:8]1[CH:9]=[C:10]([CH:13]=[C:14]([F:16])[CH:15]=1)[CH:11]=O>CO>[F:7][C:8]1[CH:9]=[C:10]([CH:13]=[C:14]([F:16])[CH:15]=1)[CH:11]=[N:1][CH:2]1[CH2:6][CH2:5][NH:4][CH2:3]1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
1.72 g (20 mmol) of 3-amino-pyrrolidine are initially introduced into 20 ml of methanol, and 2.84 g (20 mmol) of 3,5-difluorobenzaldehyde are added dropwise at 20° C., while cooling in a water bath. The mixture is subsequently stirred at room temperature for one hour and is concentrated in vacuo on a rotary evaporator, and the residue (4.5 g) is distilled. 0.9 g of an oil, boiling points 80° C.-85° C./0.04 mbar, are obtained, which decomposes to give a highly viscous mass within 4 weeks when stored at room temperature.
Workup
- additionare added dropwise at 20° C.
- temperaturewhile cooling in a water bath
- concentrationis concentrated in vacuo on a rotary evaporator
- distillationthe residue (4.5 g) is distilled
- custompoints 80° C.-85° C./0.04 mbar
- customare obtained
- customto give a highly viscous mass within 4 weeks when
- customstored at room temperature
Sources & evidence
- ORD record
- ord-823de1a11ddf4646bed4969a1e291269
- Source dataset
- uspto-grants-1997_07
- Patent number
- US05648493
Reaction notes
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