HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloromethyl Methyl Ether → HCID 19898303, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloromethyl Methyl Ether | HCID 7864 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Bispyribac | HCID 443031 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 19898303 | HCID 19898303 | 60.2% |
Reaction Steps
1.5 g (3.5 mmol) of 2,6-bis[(4.6-dimethoxypyrimidin-2-yl)oxy]benzoic acid was dissolved in N,N-dimethylformamide, and 0.1 g of 60% sodium hydride was added to the resultant solution with stirring. After the generation of hydrogen ceased, 0.4 g of chloromethylmethylether was added to the solution and the resultant mixture was reacted at 100° C. for 3 hours. After completing the reaction, ice water and ethyl acetate were added to the reaction mixture, and the ethyl acetate layer was separated and washed with water. The washed ethyl acetate layer was then dried to be concentrated, and an oily product obtained thereby was subjected to column purification to obtain 1.0 g of a white crystal having a melting point of from 95° to 96° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05114463 |
| Source dataset | uspto-grants-1992_05 |
| ORD ID | ord-a420645674a54f8b9afc5425400c2243 |
| Source note | uspto-grants-1992_05 |