HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hexane → HCID 10662594, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hexane | HCID 8058 | — |
| Reactant | 1-Bromo-2-butanone | HCID 13156 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 10611091 | HCID 10611091 | — |
| Solvent | Methyl Ethyl Ketone | HCID 6569 | — |
| Product | HCID 10662594 | HCID 10662594 | 48.2% |
Reaction Steps
A mixture of the pyridine derivative (16, 4.00 g, 15.6 m mol), 1-bromo-2-butanone (3.53 g, 23.4 m mol) and sodium hydrogencarbonate (6.55 g, 78 m mol) in methylethylketone (30 ml) was heated under reflux for 60 hours. The solid was filtered off. The volatile materials were removed by distillation under reduced pressure. The residue was chromatographed on silica gel eluting with hexane:ethyl acetate (1:2) and with ethyl acetate. The first fraction was crystallized from benzene:hexane to give 2.32 g (48.2% yield) of the titled compound 17b and, mp, 117-119° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06645976B1 |
| Source dataset | uspto-grants-2003_11 |
| ORD ID | ord-4b2a20c6508c41f5a6cd96a8b52f6053 |
| Source note | uspto-grants-2003_11 |