Reaction equation
[C:1]([OH:6])(=[O:5])[C:2]([CH3:4])=[CH2:3].[CH3:7][P:8](Cl)Cl.Cl.[OH2:12]>>[CH3:7][P:8]1(=[O:12])[CH2:3][CH:2]([CH3:4])[C:1](=[O:6])[O:5]1Participants
5
Procedure
86 g (1 mol) of methacrylic acid were added dropwise to 117 g (1 mol) of methyldichlorophosphine at a temperature from 40° to 45° C. The mixture was stirred for 1 hour at said temperature. Phosphinic-carboxylic acid dichloride was then decomposed with 18 ml of H2O at a temperature of from 40° to 60° C., whereby a considerable formation of hydrogen chloride occurred. The residual quantity of hydrogen chloride in the reaction mixture was removed in a water-jet vacuum at 150° C. The residue was distilled under reduced pressure. 126 g of 2,4-dimethyl-2,5-dioxo-1,2-oxa-phospholane were obtained, which corresponds to a yield of 85.1% of the theory.
Workup
- customThe residual quantity of hydrogen chloride in the reaction mixture was removed in a water-jet vacuum at 150° C
- distillationThe residue was distilled under reduced pressure
Sources & evidence
- ORD record
- ord-d78f1698f1174c1c952caee3554ced35
- Source dataset
- uspto-grants-1977_08
- Patent number
- US04045480
Linked notes
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