HuagongsheHuagongshe Chemistry Print Report · For research reference only
O-Methylhydroxylamine hydrochloride → HCID 57377783, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | O-Methylhydroxylamine hydrochloride | HCID 521874 | — |
| Reactant | HCID 86667097 | HCID 86667097 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 57377783 | HCID 57377783 | 89.9% |
Reaction Steps
To a solution of 0.241 g 5-(3,4-dichloro-phenyl)-6-(2,2,2-trifluoro-ethoxy)-N-(3,3,3-trifluoro-2-oxo-propyl)-nicotinamide in ethanol was added 0.051 g O-methylhydroxylamine hydrochloride and the mixture was kept at ambient temperature for 18 h. The mixture was then heated to reflux for 4 h. The clear reaction mixture was diluted with ca 2 ml water and concentrated under aspirator vacuum whereby crystallisation occurred. The product was collected by filtration and washed with water and dried to constant weight under high vacuum to yield 0.23 g of the title compound as white crystals melting at 124-126° C. MS (EI): 502.1 (M−H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08669254B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-c263723f447b442a815c91d972fd1923 |
| Source note | uspto-grants-2014_03 |