HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trichloroacetyl chloride → HCID 91021533, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trichloroacetyl chloride | HCID 6420 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 91496015 | HCID 91496015 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 91021533 | HCID 91021533 | 51.4% |
Reaction Conditions
| Temperature | 2.5 °C |
|---|
Reaction Steps
The above amide (490 mg) and triethylamine (0.37 ml) in dichloromethane (10 ml) was treated dropwise with trichloroacetyl chloride (0.16 ml) in dichloromethane (10 ml) with stirring at 0-5° C. After 0.5 h, more trichloroacetyl chloride (0.8 ml) was added and stirring continued for 0.25 h. The reaction mixture was washed with aqueous sodium bicarbonate solution, dilute hydrochloric acid, water, then brine, and dried (MgSO4). The solvent was evaporated and the residue was purified by chromatography (silica gel, dichloromethane as eluent) to give 1,1-dimethylethyl {[3-(5-chloro-2-cyanophenoxy)phenyl]methyl}carbamate (240 mg) as a colourless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07276528B2 |
| Source dataset | uspto-grants-2007_10 |
| ORD ID | ord-32031b4d3d9f41f3b4615b7d1fa146ff |
| Source note | uspto-grants-2007_10 |