HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 54348800, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | HCID 11482929 | HCID 11482929 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 54348800 | HCID 54348800 | 76% |
Reaction Steps
6 g of butyl 4,4,4,2-tetrachloro-butanoate (22.4 mmoles) in 20 ml of anhydrous toluene are charged under inert gas into a 250 ml flask and 5 ml of 1,8-diazabicyclo[5.4.0]undecan-7-ene (DBU) are added with exothermy. The mixture is brought to 60° C. for 3 hours. Upon GC control, it is observed that the reaction is complete; the mixture is cooled, water is added, the mixture is extracted with ethyl ether and anhydrified on Na2SO4. The residue obtained after evaporation of the solvent and purification by silica gel chromatography (eluant: hexane/ethyl acetate=9/1) weighs 4 g (76% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07449528B2 |
| Source dataset | uspto-grants-2008_11 |
| ORD ID | ord-773c91154cef416fac4a13f6a1423cd3 |
| Source note | uspto-grants-2008_11 |