Chloromethyl Methyl Ether → HCID 23116091, compound
Reaction equation
[CH:1]([N:4]1[CH2:8][CH2:7][CH2:6][CH2:5]1)([CH3:3])[CH3:2].[CH3:9][O:10][CH2:11][Cl:12]>CC(=O)CC>[Cl-:12].[CH3:9][O:10][CH2:11][N+:4]1([CH:1]([CH3:3])[CH3:2])[CH2:8][CH2:7][CH2:6][CH2:5]1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
A 40.00 g quantity of N-isopropylpyrrolidine was dissolved in 361 g of dehydrated 2-butanone (reagent, product of Wako Pure Chemical Ind. Ltd.), followed by replacement with nitrogen. To the solution was added dropwise 28.76 g of chloromethyl methyl ether (reagent, product of Tokyo Kasei Co., Ltd. as purified by distillation) at 5° C. over a period of 0.5 hour. The mixture was thereafter heated to a gradually elevated temperature and stirred at room temperature for 10 hours, whereby the reaction was terminated. The reaction mixture was cooled to 5° C., and the resulting solids were filtered off in nitrogen. The filter cake was washed with 200 ml of 2-butanone and thereafter dried in a vacuum, giving 66.40 g of the desired product.
Workup
- temperatureThe mixture was thereafter heated to a gradually elevated temperature
- customwhereby the reaction was terminated
- temperatureThe reaction mixture was cooled to 5° C.
- filtrationthe resulting solids were filtered off in nitrogen
- washThe filter cake was washed with 200 ml of 2-butanone
- customdried in a vacuum
Sources & evidence
- ORD record
- ord-1638ddee4e6142249b08065394a43bb1
- Source dataset
- uspto-grants-2014_06
- Patent number
- US08747690B2
Reaction notes
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