Chloroform → 3,3-Dichloropiperidin-2-one
Reaction equation
[C:1]1(=[O:7])[NH:6][CH2:5][CH2:4][CH2:3]C1.P(Cl)(Cl)(Cl)(Cl)Cl.[CH:14]([Cl:17])(Cl)[Cl:15]>>[Cl:15][C:14]1([Cl:17])[CH2:3][CH2:4][CH2:5][NH:6][C:1]1=[O:7]Participants
4
Procedure
Part A. To valerolactam (5.6 g, 55 mmol) in CHCl3 was added PCl5 (34.6 g, 166 mmol) and the reaction was heated to reflux 24 h. The reaction was cooled, quenched with H2O, extracted with CHCl3 and dried (MgSO4) to afford crude 3,3-dichloro-2-piperidinone.
Workup
- temperaturethe reaction was heated
- temperatureto reflux 24 h
- temperatureThe reaction was cooled
- customquenched with H2O
- extractionextracted with CHCl3
- dry with materialdried (MgSO4)
Sources & evidence
- ORD record
- ord-94bda8a7855946abbd901a19596d9257
- Source dataset
- uspto-grants-2006_02
- Patent number
- US06995172B2
Reaction notes
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