HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Aminoadamantane hydrochloride → 2-Isocyanatoadamantane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Aminoadamantane hydrochloride | HCID 25331 | — |
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-Isocyanatoadamantane | HCID 12882630 | 75% |
Reaction Steps
A vigorously stirred mixture of 2-aminoadamantane hydrochloride (5.01 g, 26.7 mmol), CH2Cl2 (50 mL) and satd aq NaHCO3 (50 mL) was cooled in an ice bath. After 15 min, solid triphosgene (2.64 g, 8.9 mmol) was added. The mixture was stirred in the ice bath for 30 min and the layers were separated. The aqueous layer was extracted with CH2Cl2 (100 mL). The combined organic layers were washed with brine (50 mL), dried over MgSO4 and concentrated under reduced pressure to afford the title compound (3.55 g, 75%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08828985B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-a4c317ed86d34d8ea3cd71d10c35d13c |
| Source note | uspto-grants-2014_09 |