HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl Chloride → 6-(2,4-Dimethoxybenzoyl)-(6H)-dibenz[c,e][1,2]-oxaphosphorin 6-oxide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl Chloride | HCID 6327 | — |
| Reactant | 2,4-Dimethoxybenzoyl chloride | HCID 2734719 | — |
| Reactant | 6-methoxy-(6H)-dibenz[c,e][1,2]-oxaphosphorin | HCID 11436148 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 6-(2,4-Dimethoxybenzoyl)-(6H)-dibenz[c,e][1,2]-oxaphosphorin 6-oxide | HCID 14366288 | — |
Reaction Conditions
| Temperature | 110 °C |
|---|
Reaction Steps
35.1 g (0.175 mol) of 2,4-dimethoxybenzoyl chloride were warmed to 70° C. under a nitrogen atmosphere. 40.3 g (0.175 mol) of 6-methoxy-(6H)-dibenz[c,e][1,2]oxaphosphorin were added dropwise in the course of two hours while stirring. The temperature was then slowly increased to 110° C. It was kept at this temperature until evolution of methyl chloride could no longer be detected. After cooling to 60° C., 70 ml of toluene were added. After crystallization, 50 g (75% of theory) of the abovementioned compound of melting point 112° to 115° C. were obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05096935 |
| Source dataset | uspto-grants-1992_03 |
| ORD ID | ord-a4abe4278b5547bf9a6693bb97c0f528 |
| Source note | uspto-grants-1992_03 |