HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 53935668, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Benzylamine | HCID 7504 | — |
| Reactant | HCID 57271532 | HCID 57271532 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 53935668 | HCID 53935668 | 56% |
Reaction Steps
To a solution of the product from Method E (0.10 g, 0.22 mmol) in dioxane (2 mL) was added glacial acetic acid (0.038 mL, 0.66 mmol) and benzylamine (approx. 1 mL, excess). The resulting solution was warmed to reflux for 1 hour, cooled to ambient temperature and diluted with water. The solution was extracted with ethyl acetate and the combined organics were dried over magnesium sulfate (MgSO4), filtered and concentrated. Chromatography on silica gel, followed by recrystallization from methylene chloride/hexanes gave the title compound (0.068 g, 56%). m.p. 183-184° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06403587B1 |
| Source dataset | uspto-grants-2002_06 |
| ORD ID | ord-91f212f21469405080af9e6dd776aaad |
| Source note | uspto-grants-2002_06 |