HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 57748865, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 178440679 | HCID 178440679 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 57748865 | HCID 57748865 | 80.3% |
Reaction Steps
A solution of 250 mg (1.236 mmol) of 6-tert-Butyl-quinoxalin-2-ol in 1.07 mL (11.43 mmol) phosphorus oxychloride under nitrogen was heated at 110° C. for 3 h. The solution was cooled to room temperature and added drop wise to water (10-15° C.). Ethyl acetate was added. The aqueous layer was extracted with ethylacetate. The combined organic phases were washed with water, dried over Na2SO4 and concentrated. The crude compound was purified with flash column chromatography on silica eluting with a gradient formed from n-heptane and ethyl acetate to provide 219 mg (80.3%) of the title compound as a green solid. MS(m/e): 220 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07897627B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-123d060285ba4e2996a242187ccf78c6 |
| Source note | uspto-grants-2011_03 |