HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylacetamide → HCID 178525495, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylacetamide | HCID 31374 | — |
| Reactant | HCID 178498741 | HCID 178498741 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,3-Propanediol | HCID 10442 | — |
| Product | HCID 178525495 | HCID 178525495 | 16% |
Reaction Steps
A solution of the compound of Example 51 and zinc cluster catalyst (Zn4(OCOCF3)6O) (0.0019 g, 0.0020 mmol) in 1,3-propanediol (0.5 mL) and N,N-dimethylacetamide (0.5 mL) was stirred at 120° C. for 2 h then at 100° C. for 12 h. Cooled to ambient temperature, the reaction mixture was diluted with water, and the precipitate was collected by filtration. Ethyl acetate was added to the filtrate, and the precipitate was collected by filtration. Those precipitates were combined then purified by preparative HPLC to afford the titled compound as solid (0.0067 g, y. 16%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08742113B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-4a7bfe0013ba4480904e855578a97f96 |
| Source note | uspto-grants-2014_06 |