1-Methylimidazole → HCID 178462727, compound
Reaction equation
[CH3:1][N:2]1[CH:6]=[CH:5][N:4]=[CH:3]1.[I:7][CH2:8][CH3:9]>>[I-:7].[CH2:5]([N+:4]1[CH:9]=[CH:8][N:2]([CH3:1])[CH:3]=1)[CH3:6]Participants
Procedure
200 mmol of 1-methylimidazole was taken in a round bottom flask and sealed with a rubber septum. To this, 100 mmol of iodoethane were added drop-wise over a period of one hour using a syringe. The contents in the flask began to bubble rapidly and turned light yellowish in color. The reaction flask was deoxygenated with dry nitrogen gas for about 15 min. The reaction was carried out at 80° C. for 2 days, under an inert nitrogen atmosphere. The contents were then precipitated drop-wise in cold diethyl ether and a white powder settled down. The ether phase was decanted and the contents were dissolved in chloroform, reprecipitated in ether several times, filtered, and dried in a vacuum oven at 50° C. The final product was a light yellowish powder.
Workup
- customsealed with a rubber septum
- customto bubble rapidly
- customThe reaction flask was deoxygenated with dry nitrogen gas for about 15 min
- customThe contents were then precipitated drop-wise in cold diethyl ether
- customThe ether phase was decanted
- dissolutionthe contents were dissolved in chloroform
- customreprecipitated in ether several times
- filtrationfiltered
- customdried in a vacuum oven at 50° C
Sources & evidence
- ORD record
- ord-6a9ad4f30c9e43f98c9345e74d7147b2
- Source dataset
- uspto-grants-2016_03
- Patent number
- US09293786B1
Reaction notes
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