HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formaldehyde → (2-Azabicyclo[2.2.1]hept-5-en-2-yl)acetonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Cyclopentadiene | HCID 7612 | — |
| Reactant | Aminoacetonitrile hydrochloride | HCID 11491918 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (2-Azabicyclo[2.2.1]hept-5-en-2-yl)acetonitrile | HCID 19101380 | — |
Reaction Steps
A solution of aminoacetonitrile hydrochloride (18.5 g, 0.20 mol) in water at 5° C. is treated with 37% formalin (23.0 g, 0.28 mol formaldehyde) followed by cyclopentadiene (26.0 g, 0.4 mol), stirred at 5°-10° C. for 30 minutes and diluted with methylene chloride. The phases are separated, the aqueous phase is extracted with methylene chloride and basified to pH >12 with 10% NaOH. The aqueous basic phase is extracted with methylene chloride. The methylene chloride extract of the basic aqueous phase is concentrated in vacuo to give the title product (N-cyanomethylazanorbornene), 22.7 g, which can be distilled at 68°-70° C./0.55 torr. The compound is identified by NMR and mass spectral analyses.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05284970 |
| Source dataset | uspto-grants-1994_02 |
| ORD ID | ord-999ca333a69d48c5b13f029b14914a50 |
| Source note | uspto-grants-1994_02 |