HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Chlorophenoxyacetyl chloride → HCID 66802536, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Chlorophenoxyacetyl chloride | HCID 77771 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 71492232 | HCID 71492232 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 66802536 | HCID 66802536 | — |
Reaction Steps
To a solution of Example 1 (135 mg, 0.41 mmol) in 1,4-dioxane (15 mL) were added N,N-diisopropylethylamine (169 μL, 1.02 mmol) and 4-chlorophenoxyacetyl chloride (0.45 mmol). The reaction mixture was stirred at room temperature overnight. The reaction mixture was diluted with dichloromethane and the organic layer was extracted several times with water. The combined organic layers were evaporated in vacuo and the crude residue was purified by silica gel flash chromatography, the mobile phase being a mixture of methanol and dichloromethane (in a ratio gradually ranging from 0.5% to 1% methanol in dichloromethane), yielding the title compound as a white powder. MS (m/z) 498 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09227984B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-822e3bd1f139414fae95d0a29357e999 |
| Source note | uspto-grants-2016_01 |