1-Methylpyrrolidine → HCID 16710845, compound
Reaction equation
[CH3:1][N:2]1[CH2:6][CH2:5][CH2:4][CH2:3]1.[CH3:7][Al:8]([CH3:10])[CH3:9]>>[CH3:7][Al:8]([CH3:10])[CH3:9].[CH3:1][N:2]1[CH2:6][CH2:5][CH2:4][CH2:3]1Participants
Procedure
Colorless 1-methylpyrrolidine, 212 g (2.5 mol), was added dropwise to 144 g (2 mol) of trimethylaluminum at room temperature under nitrogen gas flow with stirring. After the addition of 1-methylpyrrolidine was completed, the resulting mixture was stirred for 6 hours at room temperature to complete the reaction. 1-Methylpyrrolidine trimethylaluminum was obtained after completion of the reaction and was dried under vacuum at about 45° C. to give 300 g of a colorless liquid. The dried colorless liquid was distilled under vacuum (10−2 torr) at 600° C., during which a colorless distillate was condensed inside a vessel cooled with dry ice. This first colorless distillate was purified according to the same procedure at 60° C. to give 267 g of the colorless and highly purified 1-methylpyrrolidine trimethylaluminum.
Workup
- stirringthe resulting mixture was stirred for 6 hours at room temperature
- customthe reaction
Sources & evidence
- ORD record
- ord-b2f81f9806f145eaa0f9f9ed82ae567d
- Source dataset
- uspto-grants-2002_12
- Patent number
- US06500250B1
Reaction notes
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