HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 58137266, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | Methyl 4-hydroxyadamantane-1-carboxylate | HCID 3741502 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58137266 | HCID 58137266 | 272.7% |
Reaction Steps
A stirred solution of methyl 4-hydroxyadamantane-1-carboxylate (1.01 g, 4.8 mmol) and pyridine (0.38 mL, 4.8 mmol) in CH2Cl2 (25 mL) was cooled in an ice bath and a solution of triphosgene (0.48 g, 1.6 mmol) in CH2Cl2 (10 mL) was added dropwise over 15 min. The ice bath was allowed to melt and the mixture was stirred for 3 h at rt.* The mixture was evaporated to dryness and the residue was triturated with EtOAc (100 mL). The filtrate was concentrated to afford 1-(methoxycarbonyl)-4-adamantyl chloroformate (1.19 g, 91%) as an oil. [* In some experiments the solution of 1-(methoxycarbonyl)-4-adamantyl chloroformate was used directly.]
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09163012B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-c22fe00ba94d4b58b6e0adb51f7e2652 |
| Source note | uspto-grants-2015_10 |