HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Bromopropionic acid → HCID 89377411, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Bromopropionic acid | HCID 11553 | — |
| Reactant | 5-Methyl-3H-pyrazol-3-one | HCID 19897312 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 89377411 | HCID 89377411 | 22% |
Reaction Steps
To a solution of 3-methyl-pyrazol-5-one (5.7 g, 58.0 mmol) in anhydrous 1,4-dioxane was added 3-bromopropionic acid, and the resulting mixture was heated to reflux for 48 h.12 The reaction mixture was concentrated under reduced pressure, and the crude product was purified by column chromotography using 5-10% MeOH/DCM as an eluent to give 3j (22%) as a solid.13 mp: 210-215° C. (Lit. mp 178-180° C.); 1H NMR (400 MHz, CDCl3): δ 2.21 (s, 3H), 2.76 (m, 2H), 3.14 (s, 2H), 4.14 (m, 2H), 8.01 (brs, 1H); HRMS (m/z): [M−H]− calcd for C7H4N2O3, 169.0619; found, 169.0622.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09005670B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-85371d4e8ed847528cc3a12b83fb546c |
| Source note | uspto-grants-2015_04 |