Dichloromethane → HCID 86736268, compound
Reaction equation
[C:1]([O:6][CH2:7][CH2:8]O)(=[O:5])[C:2]([CH3:4])=[CH2:3].C(N(CC)CC)C.C(Cl)[Cl:18]>>[Cl:18][C:1]([OH:6])=[O:5].[C:1]([O:6][CH2:7][CH3:8])(=[O:5])[C:2]([CH3:4])=[CH2:3]Participants
Conditions
- Temperature
- -15 °C
Procedure
A solution of 50 cm3 of phosgene (0.7 mol) in 100 cm3 of methylene chloride was prepared in a one liter four-necked round-bottomed flask provided with a dry ice cooler, a thermometer, a mechanical stirrer and a dropping funnel. A mixture comprising 65 g (0.5 mol) of 2-hydroxyethyl methacrylate and 51 g (0.5 mol) of triethylamine in 100 cm3 of methylene chloride was added to this solution, cooled to -15° C. After one hour of stirring at 0° C., the excess phosgene was removed by bubbling nitrogen. The reaction mixture was then washed in the cold with acidified water, and then with pure water. After drying the organic phase over sodium sulphate and evaporating the solvent under reduced pressure at 30° C., ethyl methacrylate chloroformate was obtained in a yield of 96%.
Workup
- customthe excess phosgene was removed
- customby bubbling nitrogen
- washThe reaction mixture was then washed in the cold with acidified water
- dry with materialAfter drying the organic phase over sodium sulphate
- customevaporating the solvent under reduced pressure at 30° C.
Sources & evidence
- ORD record
- ord-2a5ecd3d365b4594a9e09cd41de1c3c9
- Source dataset
- uspto-grants-1979_01
- Patent number
- US04137253
Reaction notes
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