1-Methylpyrrolidine → HCID 18371946, compound
Reaction equation
[CH3:1][N:2]1[CH2:6][CH2:5][CH2:4][CH2:3]1.[CH2:7]([Al:9]([CH2:12][CH3:13])[CH2:10][CH3:11])[CH3:8]>>[CH2:7]([Al:9]([CH2:12][CH3:13])[CH2:10][CH3:11])[CH3:8].[CH3:1][N:2]1[CH2:6][CH2:5][CH2:4][CH2:3]1Participants
Procedure
Colorless 1-methylpyrrolidine, 195 g (2.3 mol), was added dropwise to 228 g (2 mol) of triethylaluminum at room temperature under nitrogen gas flow with stirring. After the addition of 1-methylpyrrolidine was completed, the resulting mixture was stirred for about 6 hours at room temperature to complete the reaction. 1-Methylpyrrolidine triethylaluminum was obtained after completion of the reaction, and was dried under vacuum at about 45° C. to give a colorless liquid. The dried colorless liquid compound was distilled under vacuum (10−2 torr) at 70° 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 70° C. to give 354 g of the colorless liquid 1-methylpyrrolidine triethylaluminum having high purity.
Workup
- stirringthe resulting mixture was stirred for about 6 hours at room temperature
- customthe reaction
Sources & evidence
- ORD record
- ord-6b8718d7e1324d5289f8a49cff4b055e
- Source dataset
- uspto-grants-2002_12
- Patent number
- US06500250B1
Reaction notes
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