HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Malonate → HCID 10020292, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Malonate | HCID 7761 | — |
| Reactant | 4-Chloroanisole | HCID 12167 | — |
| Reactant | 2-Methylbenzoyl chloride | HCID 70276 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Reactant | HCID 21463072 | HCID 21463072 | — |
| Solvent | 1,1,2,2-Tetrachloroethane | HCID 6591 | — |
| Product | HCID 10020292 | HCID 10020292 | — |
Reaction Steps
A mixture of 5-Chloro-2-hydroxy-2'-methylbenzophenone [prepared by reaction of 4-chloroanisole with ortho-toluoyl chloride in 1,1,2,2,-tetrachloroethane in the presence of aluminum chloride (150° C., 7 hours): melting point 65°-66° C.](71.9g), diethyl malonate (70 ml) and 1,8-diazabicyclo[5.4.0]undec-7-ene (4 ml) was stirred at 170° C. for 6 hours. The reaction mixture was purified by silica gel column chromatography (hexane) to yield 6-chloro-4-(2-methylphenyl)-2-oxo-2H-1-benzopyran-3-carboxylic acid ethyl ester as colorless crystals (73.2 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05700810 |
| Source dataset | uspto-grants-1997_12 |
| ORD ID | ord-154f554cd2e64c84b2d039c1cee55f54 |
| Source note | uspto-grants-1997_12 |