HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → Cyclopentadiene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 2-Chloro-N,N-dimethylethylamine | HCID 7901 | — |
| Reactant | HCID 178506819 | HCID 178506819 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Tetrahydrofuran hexane | HCID 21883165 | — |
| Product | Cyclopentadiene | HCID 7612 | — |
| Product | (N,N-dimethylaminoethyl)cyclopentadiene | HCID 12154709 | — |
| Product | Butyllithium | HCID 178418339 | — |
Reaction Steps
(2-dimethylaminoethyl) cyclopentadiene was synthesized by a modification of a literature procedure as disclosed in J. Organomet. Chem., Vol. 423, p. 31, 1992. 2-Chloro-1-(dimethylamino) ethane (43.04 g, 400 mmol) free of hydrogen chloride was added slowly to a stirred suspension of cyclopentadienyllithium in THF/hexane (1:1) (obtained from the reaction of n-butyllithium (250 ml, 1.6M in hexane) with freshly distilled cyclopentadiene (33.0 ml, 400 mmol) in THF (250 ml) at 0° C. and the reaction mixture refluxed overnight. Filtration of the lithium chloride, removal of the solvents, and a trap-to-trap distillation at reduced pressure afforded (2-dimethylaminoethyl) cyclopentadiene as a colorless liquid (53.58 g, 98%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06271322B1 |
| Source dataset | uspto-grants-2001_08 |
| ORD ID | ord-b040e015849f4f0885dfb664cfcb7ffa |
| Source note | uspto-grants-2001_08 |