HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 131723753, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-Butenoic acid, 4-bromo-, methyl ester | HCID 5369175 | — |
| Reactant | HCID 178525048 | HCID 178525048 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 131723753 | HCID 131723753 | — |
Reaction Steps
To a stirring solution of phenylmethyl 2-[(2-bromophenyl)methyl]imidazole-4-carboxylate in dimethyl foramide (0.1M) was added sodium hydride (1.2 eq) The reaction was allowed to stir for 10 mins. followed by addition of methyl 4-bromocrotonate continued stirring for 18 hr. The reaction was diluted with water and extracted with ethyl acetate. The organic layer was extracted with 10% hydrochloric acid and the aqueous layer was neutralized with saturated sodium carbonate. The aqueous layer eas extracted with ethyl acetate and dried with magnesium sulfate, filtered and concentrated in vacuo. The residue was purified by flash chromatography (50% EtOAc/Hexane). EI-MS m/z 406/408 (M+H)+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06514964B1 |
| Source dataset | uspto-grants-2003_02 |
| ORD ID | ord-8ffb09ba70d64803aa001396d00a603f |
| Source note | uspto-grants-2003_02 |