Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethyl Ether | HCID 8254 | — |
| Reactant | Ethyl Acrylate | HCID 8821 | — |
| Reactant | Dimethyl methylphosphonate | HCID 12958 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 11019721 | HCID 11019721 | 97.9% |
Reaction Steps
A flask filled with nitrogen and fitted with a cooling trap is charged with 216 g of dimethyl methanephosphonate; the contents are heated to 60° C. and a mixture of 200 g of ethyl acrylate and 100 g of methanol is added dropwise in the course of 1 hour, the temperature rising to 65° C. The reaction mixture is further stirred for 1 hour, during which period a total of 91 g of dimethyl ether are collected in the cooling trap. Excess methanol is removed by vacuum distillation. The crude product is obtained in a yield of 362 g with a 97.3% purity, which corresponds to a theoretical yield of 97.9%. The boiling point of a sample is 100°-102° C. at 0.013 mbar.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05166385 |
|---|
| Source dataset | uspto-grants-1992_11 |
|---|
| ORD ID | ord-33f874faec924ae89c4245b3a1ce986a |
|---|
| Source note | uspto-grants-1992_11 |
|---|