HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 10063713, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Potassium ethyl malonate | HCID 3446434 | — |
| Reactant | Magnesium Chloride | HCID 5360315 | — |
| Reactant | 4-Bromo-2-chlorobenzoyl chloride | HCID 15592207 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 10063713 | HCID 10063713 | 86.4% |
Reaction Steps
13bs) 6.8 g of monoethyl malonate potassium salt in 70 ml of acetonitrile were cooled to 10° under argon and treated with 5.3 ml of triethylamine and 4.8 g of magnesium chloride. The resulting thick suspension was stirred at room temperature for 2 hrs. Then, it was again cooled to 10° and 5 g of 4-bromo-2-chloro-benzoyl chloride were added dropwise thereto over 30 min. The mixture was stirred at room temperature for 15 hrs. and then concentrated. Extraction: twice with 100 ml of toluene, once with 100 ml of cold 1N HCl and twice with 100 ml of water. After drying and evaporation there were obtained 5.2 g (85%) of ethyl 3-(4-bromo-2-chlorophenyl)-3-oxo-propionate as a brown oil which crystallized in a refrigerator. M.p. 34° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05763450 |
| Source dataset | uspto-grants-1998_06 |
| ORD ID | ord-7db676c7d7454471a21c9701eed604c3 |
| Source note | uspto-grants-1998_06 |